epistemologicide (Hive Bee)
10-31-01 21:26
No 231411
      can this work  Bookmark   

originally done by madchemist, i am trying to attain a second opinion and input if any, also any knowledge on l-pheny working or not etc would be appreaciated.

There have been posts before on this subject before, but those have talked about decarboxilating it and reducing that to amphetamine.
I am going to talk about turning it into

Phenylalanine is an easy substance to get. It can be bought at any GNC store for cheap. A few hundred grams can probably be purchased for $50-$75.

The first step involed is oxidation. It is done with oxygen and a catalyst. If different catalysts are used, then different products will result.
Oxidation of phenylalanine with a copper catalyst will produce benzyl cyanide, which can be reacted with sodium ethoxide and ethyl acetate to form alpha-pheylaceto-acetonitrile. Alpha-phenylacetoacetonitrile can be reacted with H2O and H2SO4 to produce P2P.
Oxidation of phenylalanine with a silver catalyst will produce phenylacetaldehyde, which can be reacted with KMnO4 and H2SO4 to produce phenylacetic acid. Phenylacetic acid can be refluxed with acetic anhydride to produce P2P.

Since not every body has silver to make electrodes with, we will make benzyl cyanide.

Oxidation of phenylalanine can be acheived by making an electrolytic cell with a sheepskin condom and a big plastic cup. In the cup, a copper electrode (whatever you can find, pennies, copper pipe, etc..) is placed and hooked up to + 12V (car batterie). Place a graphite electrode (pencil lead) in the condom but so it isn't touching the condom. Hook it up to - 12V.
Fill the cup up with a NaOH and phenylalanine solution. Fill the condom with NaOH solution.
Let it run until the volume of oil on collecting on the bottom stops increasing. The oil is benzyl cyanide. Pipette it out and distill it with dry epsom salt to dry it.

Now that you have benzyl cyanide, you need three more things, sodium metal, ethyl acetate, and dry ethanol. We are going to make each.

First stop at a liquor store, and buy a bottle of the highest proof clear alcohol you can find, 190 proof everclear would be best, but vodka 80 proof or 100 will work.

First distill out the ethanol from the vodka or whatever. Crush up some dry epsom salt and add it to the recovered vodka, redistill to get dry ethanol.

Take some household vinegar (5%), and boil it till it is 1/8th it's originall volume. You will have a 40% acetic acid solution left. Add an equal molar amount of this to the ethanol and reflux for a few hours to produce ethyl acetate. Then you could distill out the ethyl acetate and redistill it with dry epsom to like the ethanol.

Now that you have dry ethanol, dry benzyl cyanide, and dry ethyl acetate, you need to make sodium.

Hook two iron nails to the car battery you used to oxidise the phenyalanine.
Put some NaCl into a thick glass bowl, and slowly add heat until it melts. Have a glass with mineral oil handy. Now stick the two nails into the molten NaCl. Cl- ions will be oxidised by the positive iron electrode, and Na+ ions reduced by the negative iron electrod. Beads of sodium will form on it. Scrape them off into the mineral oil as you go along.

There, now we prepare the sodium ethoxide solution.

1-Add 700cc of ethanol to a flask.
2-Cool it down in an ice bath, then slowly add 60g sodium metal with stirring.
3-When all sodium has gone into the solution, that means it has reacted to form the base sodium ethoxide, which is soluable in the rest of the ethanol. Hook up flask for reflux, and slowly heat the etoxide solution until it begins to steam and effervese lightly.
4-In a separate flask mix 2mol (234g) of dry benzyl cyanide with 3mol (264g) of dry ethyl acetate.
5-Add the benzyl cyanide solution to the ethoxide solution, and shake the flask around a little. Add a drying tube to the top of the condensor.
6-Heat the solution on a steam bath for 2 hours, then let it cool overnight.
7-Now stir it around a little to break up any clumpy materila in the flask, then remove the drying tube and condensor.
8-Cool the mix down in an ice salt acetone bath to at least -10 deg C.
9-When it hit's that temp, filter out the sodium salt. Then wash the sodium salt many times with a non-polar.
10-Precipitate alpha-phenylacetoacetonitrile by dissolving the sodium salt in 1.3 liters water, and adding conc. acetic acid. Filter out and dry.

Now that we have pheylacetoacetonitrile, it is time to make P2P.

1-Add 350mL of conc. H2SO4 to an acetone ice salt bath. Let it cool all the way down.
2-Measure out 1.3mol (206g) of the acetonitrile.
3-Measure out half of the acetonitrile's weight in water and carefully pour the H2SO4 into it. Then put the whole solution back into the ice bath and let it cool back down.
4-Slowly add the phenylacetoacetonitrile to the H2SO4 mix, keeping the temp below 20 deg C.
5-Stir rapidly, allow it to slowly come to room temp.
6-Heat slowly on a stem bath until it all goes into the solution, then cool it back down to 0C.
7-Rapidly add 1.75L of water, then heat on a rapidly boiling water bath for 2 hours, shaking here and there. Then let sit.
8-The P2P will form a layer, separate, then extract the aqueous layer with methylene chloride.
9-Wash the methylene chloride, then distill with sodium sulfate (made by reacting NaOH with H2SO4).

You know what to do with the P2P next!

hatred of ontological wastes, and the marathon!!!!
(Hive Bee)
11-02-01 00:25
No 232028
      Re: can this work  Bookmark   

You are suggesting electrolysis of molten NaCl, as a source of Sodium metal? Bad idea... The NaCl does not melt until 800 degrees C, which will make the owner of the glass bowl pretty mad. Also the sodium will float on top of the NaCl solution, allowing the oxygen in the air to oxidize it fast, as it does around 800 deg C.

How about using NaOH? That melts at around 150 degrees as i recall? I think an inert atmosphere would be nice to use in any case!

11-02-01 02:17
No 232069
      Re: can this work  Bookmark   

The meltingpoint of NaCl is 801 deg. C. I have never yet heard of anyone trying to make sodium metal from NaCl at home is the kichen or basement, I wouldnŽnt recoment it to anyone who likes to be helthy also in the future...
(Hive Bee)
11-02-01 06:01
No 232114
      Re: can this work  Bookmark   

NaOH melts at 310'C
(Hive Bee)
11-08-01 01:43
No 234515
      Re: can this work  Bookmark   

Molten lye is not the safest thing to bee near, but is do-able at home if one is careful.This is absolutely NOT a stovetop procedure, good engineering and construction technique required, but do it once and you'll be set for sodium for a LONG time.. At 300C Na will oxidize quickly, but in a closed vessel, the Hydrogen liberated will protect it from atmospheric oxygen. The Na can be ladled out with only surface oxidation ocurring during the brief transition to mineral-spirits jar.
  Dont rely on the schematic-type cell diagram in your textbook, get a look at real cells in an industrial engineering book for designs that keep the Na, H2 andO2 well separated from both each other and your heat(ignition)source. Consider argon displacement of the H2 and O2 for a garage production setup, this is how I saw it done in a home cell with concentric electrodes. Very Sano. The NaOH was melted separately, then added to the cell, and the current flow kept it fused. We had fun foolishly chucking the sodium hunks in the pond.  Again, it's  a majorly dangerous undertaking, but safe enough if you do your homework and follow proper safety protocol, this IS the serious chem forum, after all.