Preparing Urushibara catalysts , Hive Chemistry Discourse
 
    Chromic (Hive Addict) 12-22-01 20:43 No 249945       Preparing Urushibara catalysts </td> <td class="text_bg" align="right" valign="top">  <a href="https://www.the-hive.ws/forum/favorites.pl?Cat=&option=add&number=249945&Number=249945&page=81&view=&sort=5&part=&vc=&new=&backto=showflat" title="Add this post to your bookmark list in your Private Area">Bookmark</a>  </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> I heard Urushibara also made copper catalysts, and I wanted to try out their preparation (just out of curiousity, I realize they're much, much less active than the cobalt or nickel counterparts).<br><br>4g of copper sulfate pentahydrate (mw 250 g/mol, similar to nickel chloride or cobalt chloride salts used, 240g/mol) added to 75ml of water, and slowly added 5g of crumpled al foil. The solution lost its characteristic blue color and was a mixture of aluminum foil and preciptated copper, most of the foil remained unharmed.<br><br>Are all of the solids (including unused aluminum) added to 100g of 20% NaOH? Or is it just the copper that falls to the  bottom?<br><br>I'm going off of:<br><a href="http://chemistry.mdma.ch/hiveboard/rhodium/chemistry /amph.urushibara.txt" target="_blank" title="Jump to this external site">../rhodium/chemistry /amph.ur<wbr>ushibara<wbr>.txt</a> (and not the original Urushibara text)<br><br>PS. Or did I not wait long enough for all of the aluminum to dissolve in reaction with the water and dilute hydrochloric acid? </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post249998"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> uemura<br> <i>(<span title="The user's title at the time of posting">Hive Photographer</span>)</i><br> <span title="Posting date">12-22-01 23:57</span><br> <span title="Link to this post by using the markup [249998]">No 249998</span><br> </td> <td rowspan="2">  </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2">  </td> <td class="text_bg" align="left" valign="top"> <title>Re: Preparing Urushibara catalysts </td> <td class="text_bg" align="right" valign="top">  <a href="https://www.the-hive.ws/forum/favorites.pl?Cat=&option=add&number=249998&Number=249998&page=81&view=&sort=5&part=&vc=&new=&backto=showflat" title="Add this post to your bookmark list in your Private Area">Bookmark</a>  </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> Hi Chromic<br>uemura recommends to do a search! He remembers antibody posted some details and uemura also put some pics in a thread related to the urushibara cat preparation. antibody was succesfull with a 50% yield to reduce 245 tmnp to tma using the urushibara cat. <hr> Merry XMas to the Bees </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post250087"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> Antibody2<br> <i>(<span title="The user's title at the time of posting">Commodore "Mole Bouncer"</span>)</i><br> <span title="Posting date">12-23-01 10:40</span><br> <span title="Link to this post by using the markup [250087]">No 250087</span><br> </td> <td rowspan="2">  </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2">  </td> <td class="text_bg" align="left" valign="top"> <title>Re: Preparing Urushibara catalysts </td> <td class="text_bg" align="right" valign="top">  <a href="https://www.the-hive.ws/forum/favorites.pl?Cat=&option=add&number=250087&Number=250087&page=81&view=&sort=5&part=&vc=&new=&backto=showflat" title="Add this post to your bookmark list in your Private Area">Bookmark</a>  </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> chromic - yes, toss everything into the caustic activation, where most of the Al is consumed. But that will produce a useless catalyst. Check this out:<br><br>3.3. DETAILS ON INDIVIDUAL URUSHIBARA CATALYSTS<br>(a) U-Ni-A and U-Ni-B<br>Of all the Urushibara catalysts, U-Ni-A and U-Ni-B are the most<br>commonly used and have the widest applications. Either catalyst will serve for the same catalytic reduction, as there is no substantial difference in activity between the two catalysts. It sometimes happens, however, that one of them is to be preferred according to the kind and purity of the substance to be reduced, or according to the reaction conditions. Both U-Ni-A and U-Ni-B are produced from the same precipitated nickel that is deposited by the reaction between nickel salt solution and zinc dust. The precipitated nickel digested with acetic acid (or propionic acid) gives rise to U-Ni-A, and that digested with sodium hydroxide gives rise to U-Ni-B. In the latter case, the activity of the catalyst is somewhat reduced when the precipitated nickel is treated with an alkali solution of too high a concentration at too high a temperature, or when digestion is continued for a long time until the evolution of hydrogen subsides.  Highly active U-Ni-B is obtained when the precipitated nickel is warmed with an approximately 10% solution of caustic alkali for 15 minutes. It contains considerable amounts of undissolved zinc and zinc oxide. In contrast, a good result is obtained in acetic acid treatment only when digestion is continued to such an extent that the zinc and zinc compounds almost completely dissolve away, and a small portion of nickel itself is dissolved to make the solution greenish. U-Ni-A consists of 70-80% nickel, together with a small amount of zinc folded into the former, and little, if any, zinc compounds are contained in it. The same amount of precipitated nickel prepared from nickel chloride and containing 1 g of nickel metal gives rise to Urushibara catalysts of different quantities; the gross weight of U-Ni-A is 1.1 - 1.4 g (nickel content ca. 0.85 g), whereas that of U-Ni-B amounts to as much as 5-10 g (nickel content nearly 1 g), the latter being far more bulky. A neutral catalyst is readily obtained when U-Ni-A is washed a few times with water after preparation. In contrast, alkali combines with U-Ni-B so firmly that a trace amount of alkali can not be removed without much difficulty. When alkali treated precipitated nickel, which is washed twice with water and twice with ethanol, is used in catalytic reduction, the solution in which the reduction takes place be- comes weakly alkaline (pH 9-10), as indicated by the pink color of phenolphthalein. Alkali-treated precipitated nickel, which is washed 5-6 times either with water or with ethanol, makes the solution only faintly alkaline, almost neutral to phenolphthalein (pH 8-9). Trace amounts of alkali are ultimately removed only when the catalyst is washed with water ten times or more, and subsequently many times with ethanol (or other solvent to be used in the reduction process to replace the wash-water.<br>U-Ni-B is effectively employed in catalytic reductions for which the presence of alkali is favorable; whereas U-Ni-A is appropriate for those reductions where the presence of alkali interferes. For example, a trace amount of alkali favors the reduction of ketones, aldehydes, nitriles, and oximes, for which the use of U-Ni-B is desirable. On the other hand, the reduction of aromatic nitro compounds is hindered by the presence of alkali and U-Ni-A can conveniently be used in this case.<br>It is nevertheless true that U-Ni-B can be used in neutral reductions, if it is washed thoroughly with water to completely remove alkali, and U-Ni-A can be used in the same reductions that are effectively conducted in the presence of U-Ni-B, provided a small amount of alkali is added. This is compatible with the fact that the activities of these two catalysts do not differ substantially from each other.<br>The above difference in the natures of U-Ni-A and U-Ni-B is successfully applied to selective reduction. For instance, m-nitroacetophenone gives m-aminoacetophenone in good yield in the presence of U-Ni-A or thoroughly washed U-Ni-B.<br>U-Ni-A is far less bulky than U-Ni-B, and has the apparent advantage that it can be readily dispersed into solution when used in liquid phase reduction. This matters little in a reduction under atmospheric pressure, as the reaction vessel can be shaken as vigorously as necessary to obtain thorough dispersion. In a high-pressure reduction, especially in a large scale reduction in a high capacity autoclave, however, the efficiency of reduction is mainly governed by the dispersability of fine catalyst particles into the solution. In such cases, U-Ni-B has a disadvantage, and in liquid-phase reduction at high pressure the use of U-Ni-A is always preferable. Addition of an appropriate amount of alkali may, however, be required in certain cases.<br>(b) U-Ni-BA<br>U-Ni-BA is prepared by the alkali treatment of the precipitated nickel which is obtained from nickel chloride solution and aluminum, instead of zinc dust. As the preparation of the precipitated nickel in this case requires much time, it is advisable to prepare and store in advance a large quantity of precipitated nickel, from which the required amount is occasionally removed and treated with alkali.<br>The U-Ni-BA catalyst consists primarily of nickel metal, along with a small amount of contaminant, so that the bulk of the catalyst is greatly reduced, and is even smaller than that of U-Ni-A for the same nickel content.<br>The main characteristic of U-Ni-BA is its ability to hydrogenate aromatic rings of benzene and naphthalene and their derivatives. U-Ni-A and U-Ni-B can hydrogenate phenols to cyclohexanols, but are inactive to other aromatic compounds. On the contrary, U-Ni-BA is effective for almost every aromatic compound, including phenols.<br>U-Ni-BA, like U-Ni-A and U-Ni-B, can be used for the hydrogenation of olefins, or the reduction of carbonyl and nitro compounds, but it gives somewhat poorer results. We can see this in the high-pressure reduction of acetophenone. For general purposes other than for benzene ring hydrogenation, the use of U-Ni-A or U-Ni-B, with their high activity, stability, and availability is recommended.<br>(c) U-Ni-AA<br>U-Ni-AA is prepared by warming the precipitated nickel which is deposited from nickel chloride solution by aluminum grains, with acetic acid saturated with sodium chloride. It consists of aluminum grains coated by nickel, as the nickel metal deposited on aluminum grains does not separate from the latter, which remain undissolved after acetic acid treatment owing to the mild reaction between aluminum metal and acetic acid. As the aluminum grains which support the nickel metal act as a carrier, U-Ni-AA can most conveniently be used for a vapor phase reduction.<br>It is to be noted that the use of U-Ni-AA is not confined to vapor phase reduction; it is also suitable for liquid-phase hydrogenation at room temperature and atmospheric pressure. This can be seen from the reduction of nitrobenzene in ethanol which, in the presence of U-Ni-AA, gives aniline in a 70% yield.<br>(d) U-Ni-C Catalysts<br>To promote the activity of U-Ni-A or U-Ni-B, it is desirable to reduce the particle size of the catalyst so as to facilitate its dispersion into solution. U-Ni-C catalysts comply with this requirement.<br>The particle size of Urushibara catalysts is seemingly determined by that of the precipitated nickel. To reduce the particle size of the precipitated nickel, it is necessary to retard the velocity of the ion exchange reaction; that is, to retard the speed of deposition of nickel. The optimum conditions for the slow and uniform deposition of nickel on zinc dust have been established. The precipitated nickel which is prepared by the reaction of zinc dust with nickel chloride solution of an appropriate concentration, either at room temperature or with cooling by running water or ice, is treated again in the cold with acetic acid or sodium hydroxide solution. In this way we obtain U-Ni-CA and U-Ni-CB. These catalysts, compared with ordinary Urushibara nickel catalysts, have a smaller particle size and exhibit higher activity, especially for liquid-phase reduction in an autoclave. These catalysts, however, require much time for preparation, and therefore lack the distinguishing characteristic of the general Urushibara nickel catalysts namely, speed in preparation.<br>(e) U-Ni(s) Catalysts<br>Another modified preparation of Urushibara nickel catalysts consists of the addition of nickel chloride crystals, instead of a nickel chloride solution, to zinc dust mixed with a small amount of water. Owing to the heat of reaction, local reaction is promoted and precipitated nickel is formed in a few minutes. It is digested with acid or alkali in the usual way, giving rise to two kinds of catalyst. They are U-Ni-A(s) and U-Ni-B(s).<br>The extreme ease with which the precipitated nickel is produced allows the U-Ni(s) catalysts to be prepared very quickly. This ease itself might mislead one to presume that the catalysts would have impaired activities. Nevertheless, they are sufficiently active for use in almost every reduction, and their activities are very close to, although not as high as, those of ordinary Urushibara nickel catalysts. For practical purposes, they may be widely used because of their simple preparation and high activities.<br>(f) U-Ni-A(HCl)<br>The use of hydrochloric acid in the digestion of the precipitated nickel greatly reduces catalytic activity. Therefore, U-Ni-A(HCl), which is obtained by treating the precipitated nickel with hydrochloric acid, is inadequate for ordinary purposes, except in certain instances where high activity is not desirable. Though the catalyst gives fairly good results in the partial hydrogenation of acetylenic compounds (see Section 6. 5. 4), it is practically of little use because the Urushibara iron catalyst is most profitable for such partial hydrogenations.<br>U-Ni-A(HCl) and U-Ni-A(s) (HCl) may be used for the reduction of benzoin under high pressure, but their activities can not compare with those of other U-Ni-A catalysts. The cause of the impaired activity is apparently that a considerable amount of nickel is dissolved when the precipitated nickel is treated with hydrochloric acid, so that the nickel content of the catalyst is diminished, or that some chlorine compound is adsorbed on the surface of the catalyst and behaves as a kind of poison.<br>(g) U-Ni-NH3<br>Precipitated nickel also gives rise to an Urushibara nickel catalyst on treatment with aqueous ammonia instead of sodium hydroxide. This is U-Ni-NH3. A considerable amount of ammonia remains even after washing with water. Ammonia is adsorbed on the catalyst far more strongly than is sodium hydroxide on U-Ni-B.<br>Catalytic reduction of nitriles or oximes yields primary amines together with secondary amines. The use of ammonia especially favors the formation of the former. Therefore, the yields of primary amines in the catalytic reduction of these compounds are higher in the presence of U-Ni-NH3 than in the presence of U-Ni-B.<br>(h) U-Co Catalysts<br>Urushibara cobalt catalysts are modifications of the Urushibara nickel catalysts, just as Raney cobalt is a congener of Raney nickel. Their activities compare with that of Raney cobalt and have properties very similar to the corresponding useful nickel catalysts. However, they are less useful for general purposes, as their activities are somewhat less and they are more expensive. In catalytic reduction of nitriles or oximes Raney cobalt surpasses Raney nickel in depressing the formation of accompanying undesirable secondary amines. Likewise, the U-Co-B catalyst was used for the same purpose and proved to be more effective than U-Ni-B. In general, the cobalt catalysts are known to be less active than the nickel catalysts for hydrogenation of the ethylenic bond, U-Co-B can effect the selective reduction of unsaturated nitriles to unsaturated amines, leaving the ethylenic linkage intact.<br>It should be remembered that U-Co-B is entirely inactive when used in ethanol saturated with ammonia. Therefore, ammonia should be precluded from U-Co-B, even in the reduction of nitriles for which the presence of ammonia is usually preferable.<br>(i) U-Cu Catalysts<br>In general, copper catalysts have an outstanding disadvantage in hydrogenation. This is the case with the Urushibara copper catalyst, which, like the Raney copper catalyst, is far less active than the corresponding nickel or cobalt catalysts. The Urushibara copper catalyst is quite unfit for catalytic reduction under atmospheric pressure, but can be used in reduction under higher pressure, provided the reaction is carried out at a temperature higher than would be appropriate for the nickel catalyst.<br>( j) U-Fe Catalysts<br>Crystals of iron(II) or iron(III) chloride are added to zinc dust mixed with a small amount of water, affording precipitated iron which, on treatment with acetic acid, furnishes U-Fe(II) or U-Fe(III), respectively. These Urushibara iron catalysts, like the Raney iron catalyst, have a distinct specificity in favoring the partial hydrogenation of acetylenic compounds to ethylenic compounds. Either U-Fe(II) or U-Fe(III) is suitable for this purpose. It must be remembered, however, that U-Fe-BA, which is prepared from iron(III) chloride solution and aluminum grains, is completely inactive in the hydrogenation of acetylenic compounds.<br><br>check your pm, i'll send the entire document </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post250091"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> Chromic<br> <i>(<span title="The user's title at the time of posting">Hive Addict</span>)</i><br> <span title="Posting date">12-23-01 10:58</span><br> <span title="Link to this post by using the markup [250091]">No 250091</span><br> </td> <td rowspan="2">  </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2">  </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Preparing Urushibara catalysts</b> </td> <td class="text_bg" align="right" valign="top">  <a href="https://www.the-hive.ws/forum/favorites.pl?Cat=&option=add&number=250091&Number=250091&page=81&view=&sort=5&part=&vc=&new=&backto=showflat" title="Add this post to your bookmark list in your Private Area">Bookmark</a>  </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> AB2, wow, that's a pain... I was breathing in quite a bit of vapor containing NaOH, even when I cooled it by an ice bath. But if that's what needs to be done, that's easy enough. I realize the urushibara base activated aluminum precipitated copper catalyst is weak. I do have nickel and cobalt salts, but not much of each, so I wanted to experiment with the preparation of the copper catalyst first. I've about given up on the peracetic epoxidation of asarone, so I'm looking at forming the nitropropene sometime in the future... </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post250180"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> Antibody2<br> <i>(<span title="The user's title at the time of posting">Commodore "Mole Bouncer"</span>)</i><br> <span title="Posting date">12-23-01 21:19</span><br> <span title="Link to this post by using the markup [250180]">No 250180</span><br> </td> <td rowspan="2">  </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2">  </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Preparing Urushibara catalysts</b> </td> <td class="text_bg" align="right" valign="top">  <a href="https://www.the-hive.ws/forum/favorites.pl?Cat=&option=add&number=250180&Number=250180&page=81&view=&sort=5&part=&vc=&new=&backto=showflat" title="Add this post to your bookmark list in your Private Area">Bookmark</a>  </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> the best results i had with it were by precipitating Ni on Al exactly according to Ritters post "Urushibara style amphetamine" but i acid activated, which according to everyone i've spoken with is weaker than the base activated.<br><br>triied all kinds of experiments accelerating and retarding the precipitation, but none were as effective as the catalyst prepared using ritters foil proceedure. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post251113"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> Chromic<br> <i>(<span title="The user's title at the time of posting">Hive Addict</span>)</i><br> <span title="Posting date">12-29-01 08:05</span><br> <span title="Link to this post by using the markup [251113]">No 251113</span><br> </td> <td rowspan="2">  </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2">  </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Preparing Urushibara catalysts</b> </td> <td class="text_bg" align="right" valign="top">  <a href="https://www.the-hive.ws/forum/favorites.pl?Cat=&option=add&number=251113&Number=251113&page=81&view=&sort=5&part=&vc=&new=&backto=showflat" title="Add this post to your bookmark list in your Private Area">Bookmark</a>  </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> I'm in the middle of preparing a Urushibara base activated cobalt catalyst, it seems to be working the way I'd expect it to work. The characteristic pink color is lost <b>slowly</b>, where with copper it was gone almost immediately and I didn't let the aluminum to continue reacting, so what was happening, is I was pouring mostly unreacted aluminum into sodium hydroxide, which of course, is going to be a crazy violent reaction. I think for the copper catalyst, I should have heated it to 50C and left it there. I'll try that out sometime...<br><br>Except for pressurized hydrogenations, it seems that Urushibara copper catalysts aren't very valuable anyways... time to figure out an OTC prep of cobalt chloride or nickel chlorides. Gibb's energy for hydrochloric acid and nickel or cobalt is negative... given enough time/heat it should react. I'll have to try it out sometime... </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post251124"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> Chromic<br> <i>(<span title="The user's title at the time of posting">Hive Addict</span>)</i><br> <span title="Posting date">12-29-01 10:40</span><br> <span title="Link to this post by using the markup [251124]">No 251124</span><br> </td> <td rowspan="2">  </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2">  </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Preparing Urushibara catalysts</b> </td> <td class="text_bg" align="right" valign="top">  <a href="https://www.the-hive.ws/forum/favorites.pl?Cat=&option=add&number=251124&Number=251124&page=81&view=&sort=5&part=&vc=&new=&backto=showflat" title="Add this post to your bookmark list in your Private Area">Bookmark</a>  </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> Should the Urushibara cobalt catalyst turn blue? (I assume this is the cobalt dissolving in the acidic conditions) Ie does Urushibara nickel turn green?<br><br>I'm using a procedure similar to the procedure Ritter used with P2NP, except using 3/2 the molar amount of oxime to nitropropene, as it has one less oxygen to be reduced. (makes sense, right? p2np requires 6H to become amphetamine, PMP2P oxime requires 4H to become PMA)<br><br>If this reaction works, or not, it will have to win the award for best-dressed reaction. <img src="../forum/images/icons_lightgrey/cool.gif" alt="cool" title="Cool" heigth="15" width="15"><hr><font color="blue">Blue</font color="blue"><i> as in cobalt</i>... <img src="../forum/images/icons_lightgrey/wink.gif" alt="wink" title="Wink" heigth="15" width="15"> </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post251157"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> Antibody2<br> <i>(<span title="The user's title at the time of posting">Commodore "Mole Bouncer"</span>)</i><br> <span title="Posting date">12-29-01 14:28</span><br> <span title="Link to this post by using the markup [251157]">No 251157</span><br> </td> <td rowspan="2">  </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2">  </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Preparing Urushibara catalysts</b> </td> <td class="text_bg" align="right" valign="top">  <a href="https://www.the-hive.ws/forum/favorites.pl?Cat=&option=add&number=251157&Number=251157&page=81&view=&sort=5&part=&vc=&new=&backto=showflat" title="Add this post to your bookmark list in your Private Area">Bookmark</a>  </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> chromic - the urushibara nickel cholride solution is green before it has precipitated, but the final catalyst is gray-black, the darker being the prefered as the gray indicates crystalization from too vigourous a precipitation.<br><br>what color is elemental cobalt?<br><br>sure be cool if it works well on oximes, i remember reading somewhere that having NH3 present when reducing oximes favoured the formation of pimary amines, i think its even mentioned in the above excerpt somewhere. but i don't know if the oximes will dimerize under basic conditions the way the nitropropenes do. i'm thinking the NH3 might take care of the Al consumption/hydrogen generation, but again unsure.<br><br>something familiar there? </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post251179"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> <font color="#FF0033">Rhodium</font><br> <i>(<span title="The user's title at the time of posting">Chief Bee</span>)</i><br> <span title="Posting date">12-29-01 15:46</span><br> <span title="Link to this post by using the markup [251179]">No 251179</span><br> </td> <td rowspan="2">  </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2">  </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Preparing Urushibara catalysts</b> </td> <td class="text_bg" align="right" valign="top">  <a href="https://www.the-hive.ws/forum/favorites.pl?Cat=&option=add&number=251179&Number=251179&page=81&view=&sort=5&part=&vc=&new=&backto=showflat" title="Add this post to your bookmark list in your Private Area">Bookmark</a>  </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> All finely powdered (precipitated) transition metals should be black in appearance. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post251182"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> <font color="#ff0000">Osmium</font><br> <i>(<span title="The user's title at the time of posting">Stoni's sexual toy</span>)</i><br> <span title="Posting date">12-29-01 15:55</span><br> <span title="Link to this post by using the markup [251182]">No 251182</span><br> </td> <td rowspan="2">  </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2">  </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Preparing Urushibara catalysts</b> </td> <td class="text_bg" align="right" valign="top">  <a href="https://www.the-hive.ws/forum/favorites.pl?Cat=&option=add&number=251182&Number=251182&page=81&view=&sort=5&part=&vc=&new=&backto=showflat" title="Add this post to your bookmark list in your Private Area">Bookmark</a>  </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> Can sulfates be used for the catalyst preparation? </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post251190"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> Chromic<br> <i>(<span title="The user's title at the time of posting">Hive Addict</span>)</i><br> <span title="Posting date">12-29-01 16:17</span><br> <span title="Link to this post by using the markup [251190]">No 251190</span><br> </td> <td rowspan="2">  </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2">  </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Preparing Urushibara catalysts</b> </td> <td class="text_bg" align="right" valign="top">  <a href="https://www.the-hive.ws/forum/favorites.pl?Cat=&option=add&number=251190&Number=251190&page=81&view=&sort=5&part=&vc=&new=&backto=showflat" title="Add this post to your bookmark list in your Private Area">Bookmark</a>  </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> Os, sulfates can be used. All anions are washed from the catalyst with the 5x wash.<br><br>Ab2, the catalyst looked like a charcoal sludge (when wet, fine powder when dry). I wish I could find a way to prepare it on a larger scale, as it's so time-consuming to make... the problem is that the reaction is so damn exothermic and the reagents so corrosive that I don't trust myself to do it... non-hydrated cobalt salts are blue (as seen in the acidic aqueous solution), hydrated cobalt salts are pinkish-purple (as used to prepare the catalyst). The blue color I saw (and is gone now) was during the reduction of the oxime...<br><br>Rhod, the copper (transition metal) catalyst looked like a brown sludge (when wet, fine powder when dry). </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post251192"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> Antibody2<br> <i>(<span title="The user's title at the time of posting">Commodore "Mole Bouncer"</span>)</i><br> <span title="Posting date">12-29-01 16:27</span><br> <span title="Link to this post by using the markup [251192]">No 251192</span><br> </td> <td rowspan="2">  </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2">  </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Preparing Urushibara catalysts</b> </td> <td class="text_bg" align="right" valign="top">  <a href="https://www.the-hive.ws/forum/favorites.pl?Cat=&option=add&number=251192&Number=251192&page=81&view=&sort=5&part=&vc=&new=&backto=showflat" title="Add this post to your bookmark list in your Private Area">Bookmark</a>  </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> <font color="blue">>As for the soluble nickel salt, the chloride, nitrate, sulfate, and acetate were successively employed, and nickel chloride was found to be the most appropriate for obtaining a catalyst of high activity. Nickel nitrate solution hardly reacts with zinc dust, and nickel sulfate solution yields a catalyst of rather low activity. Nickel acetate, on the contrary, readily yields precipitated nickel, which proves to give as good a catalyst as that obtainable from nickel chloride.</font color="blue"><br><br>another excerpt rom hata's book </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post251198"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> Chromic<br> <i>(<span title="The user's title at the time of posting">Hive Addict</span>)</i><br> <span title="Posting date">12-29-01 16:40</span><br> <span title="Link to this post by using the markup [251198]">No 251198</span><br> </td> <td rowspan="2">  </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2">  </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Preparing Urushibara catalysts</b> </td> <td class="text_bg" align="right" valign="top">  <a href="https://www.the-hive.ws/forum/favorites.pl?Cat=&option=add&number=251198&Number=251198&page=81&view=&sort=5&part=&vc=&new=&backto=showflat" title="Add this post to your bookmark list in your Private Area">Bookmark</a>  </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> I stand corrected. I didn't think there'd be any anionic effects in the reaction. I'm surprised and confused? Any explanation why?<br>PS. (sigh) basifying the mixture smells like ammonia, not good... not good at all... oh well, you never know until you work it up. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post251214"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> <font color="#ff0000">Osmium</font><br> <i>(<span title="The user's title at the time of posting">Stoni's sexual toy</span>)</i><br> <span title="Posting date">12-29-01 17:42</span><br> <span title="Link to this post by using the markup [251214]">No 251214</span><br> </td> <td rowspan="2">  </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2">  </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Preparing Urushibara catalysts</b> </td> <td class="text_bg" align="right" valign="top">  <a href="https://www.the-hive.ws/forum/favorites.pl?Cat=&option=add&number=251214&Number=251214&page=81&view=&sort=5&part=&vc=&new=&backto=showflat" title="Add this post to your bookmark list in your Private Area">Bookmark</a>  </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> > I didn't think there'd be any anionic effects in the <br>> reaction. I'm surprised and confused? Any explanation why?<br><br>The sulfate is reduced during catalyst preparation, maybe down to the sulfide. Sulfur compounds are catalyst poisons. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post251223"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> Chromic<br> <i>(<span title="The user's title at the time of posting">Hive Addict</span>)</i><br> <span title="Posting date">12-29-01 18:48</span><br> <span title="Link to this post by using the markup [251223]">No 251223</span><br> </td> <td rowspan="2">  </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2">  </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Preparing Urushibara catalysts</b> </td> <td class="text_bg" align="right" valign="top">  <a href="https://www.the-hive.ws/forum/favorites.pl?Cat=&option=add&number=251223&Number=251223&page=81&view=&sort=5&part=&vc=&new=&backto=showflat" title="Add this post to your bookmark list in your Private Area">Bookmark</a>  </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> I added 0.8ml sulfuric to 10ml acetone, dissolved yellowish oil (smelling something like the ketone, but not strongly) in 20ml acetone, added about 1ml of the acidic acetone, white crystals swirled around, added another 3ml, they went away. <sigh> Threw it into the freezer, crystals still not there. <br><br>Maybe I should pick another hobby, alas, I will do an acid/base, just for the "fun" of it. Looks like there's less than .5g tho.. reaction was run with 2.5g of oxime. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post251271"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> Chromic<br> <i>(<span title="The user's title at the time of posting">Hive Addict</span>)</i><br> <span title="Posting date">12-29-01 21:30</span><br> <span title="Link to this post by using the markup [251271]">No 251271</span><br> </td> <td rowspan="2">  </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2">  </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Preparing Urushibara catalysts</b> </td> <td class="text_bg" align="right" valign="top">  <a href="https://www.the-hive.ws/forum/favorites.pl?Cat=&option=add&number=251271&Number=251271&page=81&view=&sort=5&part=&vc=&new=&backto=showflat" title="Add this post to your bookmark list in your Private Area">Bookmark</a>  </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> The yields were meaninglessly low, <1% (plus I have no way to confirm what I ended up with).<br><br>There was a white crystalline IPA soluble bitter (yuck, this is bitter without having the pleasant bitter taste of MDMA, this is sort of bitter tasting like tylenol...) residue left over after an acid extraction (I flooded with DCM, added water, separated, neutralized, and extracted with IPA, boiled IPA off)... The marquis reagent didn't give a distinct color change (it went a very, very light orange)... but did liberate HCl (so I doubt it being the oxime). Oh well. Gotta try anything once.. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post251317"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> halfapint<br> <i>(<span title="The user's title at the time of posting">Ubiquitous Precursor Medal Winner</span>)</i><br> <span title="Posting date">12-30-01 02:32</span><br> <span title="Link to this post by using the markup [251317]">No 251317</span><br> </td> <td rowspan="2">  </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2">  </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Preparing Urushibara catalysts</b> </td> <td class="text_bg" align="right" valign="top">  <a href="https://www.the-hive.ws/forum/favorites.pl?Cat=&option=add&number=251317&Number=251317&page=81&view=&sort=5&part=&vc=&new=&backto=showflat" title="Add this post to your bookmark list in your Private Area">Bookmark</a>  </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> I was not able to sucessfully precipitate nickel onto aluminum grains from a nickel nitrate solution, even above 70<sup>o</sup>. I had to convert everything to the chloride. After that, the rxn was properly exothermic and went as advertised, though I let the temp climb up near 50<sup>o</sup>. I find it most convenient to store the dried catalyst on the aluminum grains.<br><br>I have used this form of the catalyst in alkaline solution (of a nitropropene), to generate hydrogen in situ, by the reaction of the aluminum. I would then add aluminum filings when hydrogen generation slowed. Sometimes I think I cut too many corners --- but then I look at Ritter's simplified method, and then I feel better.<br><hr>turning <b>science fact</b> into <b><i><font color="red"><<science fiction>></font color="red"></i></b> </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post251351"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> Antibody2<br> <i>(<span title="The user's title at the time of posting">Commodore "Mole Bouncer"</span>)</i><br> <span title="Posting date">12-30-01 09:21</span><br> <span title="Link to this post by using the markup [251351]">No 251351</span><br> </td> <td rowspan="2">  </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2">  </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Preparing Urushibara catalysts</b> </td> <td class="text_bg" align="right" valign="top">  <a href="https://www.the-hive.ws/forum/favorites.pl?Cat=&option=add&number=251351&Number=251351&page=81&view=&sort=5&part=&vc=&new=&backto=showflat" title="Add this post to your bookmark list in your Private Area">Bookmark</a>  </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> just to make sure i understood you correctly HP, it was basic media the hydrogenation was run in, not just the activation? any success? </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post251369"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> Chromic<br> <i>(<span title="The user's title at the time of posting">Hive Addict</span>)</i><br> <span title="Posting date">12-30-01 11:36</span><br> <span title="Link to this post by using the markup [251369]">No 251369</span><br> </td> <td rowspan="2">  </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2">  </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Preparing Urushibara catalysts</b> </td> <td class="text_bg" align="right" valign="top">  <a href="https://www.the-hive.ws/forum/favorites.pl?Cat=&option=add&number=251369&Number=251369&page=81&view=&sort=5&part=&vc=&new=&backto=showflat" title="Add this post to your bookmark list in your Private Area">Bookmark</a>  </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> Ahh, much cooler idea. I bet I might have accidentally performed a Beckmann rearrangement on the oxime and apparently I also hydrolysised it back to ketone/hydroxylamine (I should have thought about what I was trying to do, rather than to go ahead and do it..), rather than a reduction...<br><br>Basic generation of insitu hydrogen would be a good idea... I guess I should read the whole urushibara text. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post251924"></a><a name="last"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> foxy2<br> <i>(<span title="The user's title at the time of posting">Distinctive Doe</span>)</i><br> <span title="Posting date">01-02-02 00:24</span><br> <span title="Link to this post by using the markup [251924]">No 251924</span><br> </td> <td rowspan="2">  </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2">  </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Preparing Urushibara catalysts</b> </td> <td class="text_bg" align="right" valign="top">  <a href="https://www.the-hive.ws/forum/favorites.pl?Cat=&option=add&number=251924&Number=251924&page=81&view=&sort=5&part=&vc=&new=&backto=showflat" title="Add this post to your bookmark list in your Private Area">Bookmark</a>  </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> <blockquote title="Quoted text"><hr><p>I guess I should read the whole urushibara text. <p><hr></blockquote><p><br><br>LOL<br><hr>Foxy STILL needs to get laid!!! </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> </body> </html>