Author Topic: Ephedrine O-Phosphate -> Meth  (Read 1582 times)

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Rhodium

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Ephedrine O-Phosphate -> Meth
« on: April 11, 2004, 06:33:00 PM »
L-, D-, and DL-Ephedrine Phosphates
A. Larizza, G. Brancaccio, A. Segre

J. Med. Chem. 9, 966-967 (1966)

(https://www.thevespiary.org/rhodium/Rhodium/pdf/meth.ephedrine.phosphate.pdf)

Reaction of L-Ephedrine with POCl3 gave L-2-Chloro-3,4-dimethyl-5-phenyl-1,3,2-oxazophospolidine 2-oxide, which upon hydrolysis yielded L-Ephedrine O-phosphate Hydrochloride. Catalytic hydrogenation of 2.8g of the ester salt using 0.28g 5% Pd-C (2h, 1 atm, 22°C) in 40 mL ethanol gave, after filtration, acid/base extraction and distillation of the freebase (bp 91-93°C/15 mmHg) 1.2 grams of product amine (84% yield).


Aurelius

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Title
« Reply #1 on: April 12, 2004, 12:30:00 PM »
Rhodium, you should specify that it is from O-phosphate ester of ephedrine.  The title could imply the amine salt.  (which is how I read it coming into the thread.)

However, a very nice procedure with decent yield!  What search path yielded this nugget? (key words that you used in what database- if you can tell such things)


Rhodium

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Synthetic Reductions in Clandestine Labs
« Reply #2 on: April 12, 2004, 01:42:00 PM »
It's from the reference list at the end of

https://www.thevespiary.org/rhodium/Rhodium/chemistry/amphetamine.reduction.html



I'm trying to link up the entire reference list to the original literature (or the pertinent sections from the referenced article).