tpower9s2003 (Newbee)
08-06-03 02:58
No 452073
      Trying to find the best way.....some advice  Bookmark   

SWIT has already done lots of reading on extractions and so fourth. His interest lies in freebase as doing a cook in stealth might mean having to keep cook times a little shorter than HCL would demand (though at least 15hrs wouldnt be a prob), as well as the rumors of better final yields and a cleaner post fluid likely when of the more nano-scaled RP/I2 type.

SWIT hasn't attempted an STB as its yields seems low compared to the STE (a newer method, but that would be HCL, not FB) and also seems it probably would not clean the available pills as well, ALL of which found (checked the shiny NDMF 30s/several types NDMF 60s/DMF 120s) having the newer and nastiest oranges. Even an STE alone doesn't always get every last bit.  

Was wondering opinions on this:
Could SWIT do the original STE exactly, then FB the PFED HCL using RDL NaOH, dried washing soda, non-iodized NACL, research grade activated carbon, dry acetone, very minimal DH20, like the combo used for STB. To extract pull with heated till boiling dry VM&P a couple times, decant through a single coffee filter to keep any of those insoluble freebasing ingrediants from possible contamination (no need to focus on getting out gaaks the STE already got practically all of). Then evaping the combined Naptha pulls to reveal the FB ready for rxn. Seems the older STBs main yield killers would be mechanical ones related particularly to the needed fine filtering and additional heating/recryst steps normally used to get rid of gaaks. Also, since it involves FB the fully gaaked pill mass and pulling from that with just the natha, obviously yield will fall short of newer combos of the STE.

In any case, SWIT is pretty sure the result of doing the FB BEFORE an STE would not work out so well from differeing properties of FB to HCL and what he mentioned before, not completely sure if its all right.

It does just seems that FB of a clean HCL would more insure a complete conversion and easy clean pull yielding close to 100% of available FB out of the cleaned HCL. If SWIT is onto something that would work out well here, this would mean STE yields and cleaning power with any additional cleansing in the FB liberation also probably eliminating that pre-STE TCE wash saving some yield. Any recommendations? Does this sound good to go?

"True love" is a thrill
Add a methyl group or two
Get it in a pill!
(Hive Bee)
08-06-03 04:26
No 452078
      I have done it ...  Bookmark   

I have done what you are proposing with toluene in the past.  I just let it evap and then washed the fb crystals with dh20.
Doing it the way you are suggesting will give you a very clean fb, provided the STE works with your pills.  Whether or not its worth the extra time and effort is the questtion.
Why do you think the fb will be faster than the hcl?
Since it is slightly cleaner then it may be a little easier to reduce but i doubt that it would be significant.  The fb is also much more sensitive as well and yeild will suffer if your not careful.
The fb gets change to the salt as soon as HI is made anyway.
If basing the hcl is also removing more gaak then i would do it.  However if not, I would consider it a waste of time.

It wasn't Me!
08-06-03 07:04
No 452094
      HCL vs FB  Bookmark   

i noticed a comment you made to geez,last nite i think on whiteflakes dirty process of extracting pseudo.
you had stated that you extract pseudo hcl with the ste and then dissolve in meoh and precip in xylene,Key word being pseudo hcl. This procedure won't work with pseudo free base will it?

MUFF divers go down deep...
(Hive Bee)
08-06-03 09:43
No 452111
      Not sure what you mean  Bookmark   

The STE will give hcl but he was going to do the STE followed by STB which gives fb.  Does that answer your ? or did I misunderstand?

Lately i have been doing the STE and then redissolving in methanol and precipitating into xylene by boiling off the methanol.

It wasn't Me!
08-06-03 10:25
No 452118
      Didnt mean to start another FB vs. HCL thread.  Bookmark   

Didnt mean to start another FB vs. HCL thread. SWIT read the recent thread comparing the 2 and some others and from what he could gather, it might reduce more completely under the same conditions, given it wasn't accidently burned. He doesn't think cold starting a wetter reflux (g PFED to ml DH20) maybe in a prechilled rxn vessel and an oil bath, also starting cold with a 40w clear appliance bulb, not a high powered hot plate (nevertheless this can still get into the 150C range), would cause it to burn. In the given condition seems as though FB might be worth the extra effort as it would be even cleaner than the STE outcome. With the available pills, STE will get them pretty clean done carefully (minor foil discoloration where it was burned and no residual greasiness etc on foil test), though the DMF 120s are harder to get decent yields with being very finicky about the most trace amounts of DH20.

SWIT has to continue drying the 91% IPA with the dry Napth. Doesnt even measure the NaCL/dried Calcium carb, it takes A LOT so he eyes out what is surely >5g each per box equivelent as hes got KILOs of both. Either way, it gets it pretty dry, dry enough for any the NDMFs to work fine. He did try what seemed it would have to be dry (a claimed pure IPA gas line cleaner). The other, though non H20 ingredients mustve made up A LOT OF IT, as it formed 2 seemingly dry layers with Napth. Since thats not supposed to happen and the stuff doesnt give the other ingredients, hes not sure which the layers are (theyre slightly unequal in size) what bc it also became cloudy and stayed that way after fine filtering frown. He got the 91 and forgot even using that stuff. the electronics cleaner 99+ stuff available was WAAAY to expensive for IPA (like $5 bucks for only 30mL, go figure).   

On another note, SWIT opened up a cabinet in the basement way and found a seemingly unused, rugged looking piece of glassware that sure looked like a legit erlenmeyer. Forget pepper

"True love" is a thrill
Add a methyl group or two
Get it in a pill!
(Of Counsel)
08-06-03 11:48
No 452128
      Freebasing pseudo  Bookmark   

If you extract fairly clean pseudo HCl, you may freebase it with sodium carbonate and extract into any suitable nonpolar solvent. There is no need to use the salt, or for that matter the NaOH, or the carbon. The NaOH is overkill; the carbon and salt are no longer needed if the pseudo has already been extracted by a good method. To extract the freebase use naptha and freeze to precipitate or use tolulene and evaporate.

You may use water to mobilize the base if you are sure the pseudo is clean of PEG and Orange gakks. If it is not, using water to base will most likely not solve the problem.
Any good waterless a/b technique will work here, and when doing this I prefer to mix dried alcohol and dried acetone to mobilize the base to freebase the pseudo HCl. Note that if you are already orangeII gakked, the pseudo may not freebase with sodium carbonate, mobilized with the alcohol/acetone fluid or with water. I have observed this phenomenon twice now. On both occasions when sodium carbonate did not work to freebase the pseudo, orange II contamination was present. Just an observation. I have no idea about causal relationship.

I suggest that prior to freebasing the pseudo HCl you determine how clean it really is. Burn tests help. You may also note how fine and powdery the pseudo is. Clean pseudo will crumble and pour, break apart without resistance, dissolve readily. Dirty pseudo tends to clump, cling to the sides of dishes, dissolve slowly, and not crumble. If you have dirty pseudo, IPA/acetone recrystalizing helps clean it, as does the xylene clean. I have discovered that the xylene precipitation technique post Straight to E extraction will clean most remaining gakks from the pseudo HCl. whether this is due to fresh solvents or the absence of other gakks the second time around I do not know. I just know it works well.

Cleanliness of the pseudo will help improve yields. I have discovered that my yields from pseudo HCl and pseudo freebase have been equivalent in the PIE long wet reflux when the pseudo was equally clean. The real advantage to reacting the freebase form may stem as much from the better cleanliness of the freebase form as any thing else. After a couple of recrystalizations after the STE process, yields have been equivalent to yields from freebase. Yields from some pills after STE alone have been better than my best yields from freebase. I duplicated this with pseudo HCl from the same pills; I have not had the same results with any other pills to this point. This suggests that the cleanliness of the pseudo, whether HCL or freebase, is likely more important to yield that the form of the molecule. Freebase pseudo as a rule tends to be cleaner than most pseudo HCl extracted from pills, and that may explain why many of us report higher yields with freebase.

Mostly harmless
08-06-03 17:18
No 452172
      cleanliness is next to...  Bookmark   

laughGEEZ, That was a lot to swallow in one sitting.I understand the concept and information though. It just takes 2 or 3 reads on a subject with two closly related topics.

Heres my senaireo,as follows:

Not to be duplicating everyone's same ole statement but,i've got the cleanest pseudo fb this side of the Missisippi River.Heres why,started with perrigo-go 120's into coffee grinder for the STRAIGHT TO THE BEE extraction followed by(2)two dual solvent recrystallizations and at this point we were talkin windmill crystals freebase in the extra long pyrex baking dish about the size of a half dollar. then we took a caB STRAIGHT TO THE E FOLLOWED up with 2 more re-cry,which produced hcl salts,amazing.
AT this point, the good doctor GEEZMESTER told me how to
get back to freebase which he mentioned above with the sodium carbonate bassing dh2o and naptha and now we were talking toothpic chards,no shit
I thought this would bee suitableuntil i slowly wet refluxed 15 g's to end up with orange juice only.

of the same pseudo that i want to get the orange out.Any suggestions?

MUFF divers go down deep...
(Hive Bee)
08-06-03 19:02
No 452210
      effy--->meth in 4 hours  Bookmark   

From what I understand, you want to use freebase pseudo to
lower your cook time correct?

GAA might be the method for you
../rhodium/chemistry /meth.hi-p.html
(Stoni's sexual toy)
08-07-03 05:27
No 452281
      > i've got the cleanest pseudo fb this side  Bookmark   

> i've got the cleanest pseudo fb this side of the Missisippi River.

No you don't.

I'm not fat just horizontally disproportionate.
(Of Counsel)
08-07-03 13:34
No 452341
      waterless helps  Bookmark   

If your pill source was Perrigo 120's you have one or the other or both orange gakks. Those pills became terribly nasty earlier this year. When you freebased with water, you let the orange sneak over with the pseudo. Staying waterless with the a/b and using sodium carbonate seems to have worked for me. Re-read my comment in my post above about using a water based A/B if you are sure the pseudo is clean. Your wasn't.

Those 120's used to be my favorite source. Now they're well down the list.

Mostly harmless