Oh hi 



Dis is L-Phenylacetylcarbinol, produced by the fermentation of benzylaldehyde/dextrose/special yeasts.

Ephedrine is made from it by reductive amination.


Now,
Will it be possible to use (for example) NaBH4 or I2/RP to reduce the amine + the hydroxy group in the same reaction ?
Because reductive amination, recrystalisation and Re-reduction, recrystalisation seems to be a waste of time. Is it needed ?

Catalytic Hydrogenation. This procedure below will reduce the -OH and reductive amination.

1st step. reductive amination with Pd/BaSO4 (or 10%Pd/C) catalyst, H2 at 1 ATM pressure until imine is reduced to -NHCH3

2nd step. Reaction Mixture. Add 0.06-0.1 moles of Ephedrine.HCl to a solution of 100 mls of glacial acetic acid + 4 mls of 70 % w/w perchloric acid. Add 0.5 grams of 5-10% Pd/BaSO4 (or 10%Pd/C) catalyst.

Reaction Conditions.
H2 at 1 ATM pressure.
80-90 oC
10 minutes for Ephedrine.HCl
Stirred constantly during reduction.

Yield: 60-80%

Now you can substitute the 4 mls of 70 % w/w perchloric acid with 4 mls of con. H2SO4, however perchloric acid is better.

Since the H2 pressure is at 1 ATM, a balloon of H2 WILL have a greater pressure than 1 ATM. Make sure all O2 is vacuumed out IF you do use the ballon method.

There is no concern for "over reduction", even if you use the H2 balloon method, as the temperature and H2 pressure IS NOT at reaction reduction conditions for a Pd catalyst to hydrogenate the benzene ring.

Raney nickel. http://en.wikipedia.org/wiki/Raney_nickel

RANEY-NICKEL CATALYSTS PRODUCED BY MECHANICAL ALLOYING. http://www.ipme.ru/e-journals/RAMS/no_71808/zeifert.pdf

During the activation of the nickel-aluminium alloy to make Raney nickel, H2 gas is produced and can be stored with a balloon (vacuum all air out first) for the Catalytic Hydrogenation.

http://en.wikipedia.org/wiki/Raney_nickel#Activation

H2 gas can be make with a 1M sodium hydroxide solution and aluminium. Reaction: 2 Al + 2 NaOH + 6 H2O => 2 Na[Al(OH)4] + 3 H2

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http://www.erowid.org/archive/rhodium/chemistry/amphetamine.reduction.html