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                          Urushibura Style Amphetamine
                                   by Ritter
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First of all many thanks go to CHEM_GUY for his continuous urging of the Hive
community to try Urushibara Nickel reduction on phenylnitropene. This reduction
turned out to be easier than any so far encountered. This is not based on any of
the excellent references pertaining to Urushibara that have been mentioned on
the hive, only chem_guys postings!

Procedure:

Dissolve 4.0g Nickel Chloride hydrate (light green crystals) in 75 ml 95%
ethanol w/ mag stirring and warming to 50'C. After salt is dissolved remove stir
bar and add 1ml water and 1ml conc. HCl. [1] While solution at 50'C slowly add
5g regular Reynolds wrap torn up into .25 x 1.0in strips in 1g portions with
manual stirring. The aluminum will SLOWLY react with the nickel salt forming the
metal Ni(s) through metathesis as a dark grey chunky powder which settles to the
bottom. A gentle effervescence of hydrogen occurs during reaction. Add aluminum
at a rate that maintains a steady effervescence and keeps temperature roughly in
the 50' range. Note this may take up to two hours!

At the end of Al addition all green color from nickel salt should be discharged.
If any color remains add another gram of aluminum and wait for soln to clear.
Precipitated Nickel powder was added to 100ml 20% NaOH soln and manually stirred
at 60'C for 30 min. Excess NaOH is decanted and nickel is washed with 5 x100ml
aliquots of distilled water to remove excess base. At this point Urishubara
nickel catalyst is prepared and ready for reduction.

Dissolve 5g pure phenylnitropropene in 50ml Ethanol and add to Ni solution [2].
Now slowly add 3ml conc. HCl [3] and 1 gram shredded aluminum w/ manual
stirring. Aluminum will slowly dissolve with a more vigorous effervescence of
hydrogen than the first step. Maintaining good stirring with a glass stirring
rod is essential in beginning. Attempted magnetic stirring will result in
frustration because nickel is ferromagnetic and will stick to stirbar preventing
surface area exposure necessary for reduction. After aluminum is dissolved add
three more milliliters HCl and one more gram Al. Repeat adding acid and Al until
10 grams Al and about 30ml HCl has been added. Aluminum reacts slowly. Expect
addition to take about six hours, longer if temp falls below 50’C. Constant
stirring towards end is not necessary, just give mix a good stir occasionally.

After all aluminum is added and mostly decomposed slowly pour in a soln of 30g
NaOH in 100ml H20 with careful stirring. Wear goggles and be careful! Base
neutralization is highly exothermic! In 30 minutes all aluminum sludge will
solvate into bottom aqueous layer and a nice orange alcohol layer reeking of
amine will settle out on top. Nickel is not dissolved by the NaOH so it will
remain floating around between the two layers but this does not present a major
problem. After all, it’s not poisonous like mercury or anything! Now decant off
the top orange organic layer and distill off alcohol down to a orange stinky
syrup completely different smelling than the P2NP. Dissolve these goodies in
acetone and slowly add sulfuric acid to precipitate the amine sulfate.
Voila!!!!!! about 3 grams light yellow amphetamine sulfate.

[1] Addition of water and acid found to be necessary to initiate rxn between
    NiCl2 and Al.

[2] When nitropropene was added to NiCl2 soln before conversion to Ni powder
    was complete some polymerization occurred greatly reducing yield.
    It seems essential to add P2NP to rxn after Ni is fully precipitated.

[3] Use of Sulfuric acid produced inferior results causing polymerization of
    P2NP to red tar.

Increasing Yield: Use overhead mechanical stirring to keep nickel catalyst
                  better suspended during reduction. Re-extract aqueous NaOH/Al
                  layer w/ toluene and work up in standard manner. Use larger
                  amount of nickel catalyst and more aluminum for H2 generation.

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