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Discussion => Off topic => Topic started by: ruthenium on March 31, 2013, 03:17 am

Title: 1 step synthesis P2NP to amphetamine sulphate using Al amalgam
Post by: ruthenium on March 31, 2013, 03:17 am
Amphetamine sulphate #3
5g 1-phenyl-2-nitropropene was dissolved in 50ml hot IPA in a 400ml beaker, in the meantime 7.5g of Al foil cut into squares were thrown into 75ml 70% acetic acid and a few spatula points of HgCl2 were added and stirred for a bit, this was left standing for 10-15 minutes until hydrogen evolution was visible, then the IPA mixed solution was added and stirred a bit so it formed a homogenous solution, then left refluxing until all Al (or almost all Al :-P) was oxidised to Al(OH)3, the solution was now put on a hotplate and refluxed for 90 minutes, in the meantime a concentrated NaOH solution was made and put in the fridge, after reflux solution was allowed to cool and leftover Al and acid killed and basified to pH 13.
The top alcoholic layer was separated and the remaining slurry mixture re-extracted several times until you find it enough with IPA, the combined extracts removed in rotavap, then acidified with conc. HCl, additional water was added, basified to pH 13 with 25% NaOH, extracted with 3x 25ml DCM, the extracts were washed 1x with brine, 1x with a saturated sodium carbonate solution and finally with 2x water. The organic extracts were dried over MgSO4 and removed under vacuum again leaving the pure freebase.
The remaining freebase was dissolved in 4x it's volume of IPA, then 20% H2SO4 in IPA solution was added drop wise until pH 7 was reached, if pH got lower then 7 the amphetamine sulphate will redissolve and you will have to rebasify etc..
The salt was washed with 2x 20ml IPA and 1x 20ml ice cold anhydrous acetone and left air drying to yield 3.5g dry amphetamine sulphate (70%)

Note: you need 70% acetic acid, the water is required for hydrogen formation (after all this is a catalytic hydrogenation forming hydrogen in situ)