AMPH phosphate prep'n and bioassay! :D

joe_aldehyde · huxleys associate

swim prepared this compound by dropwise adding 85% phosphoric acid to a solution of phenylisopropylamine in dry diethylether with vigorous stirring, the formed fluffy precipitate being filtered off. freebase was purified preliminarily via 2x a/b extraction. due to improper conditions, phosphate and hydrogenphosphate salts also formed to a considerable extent which are hygroscopic and were slightly pink, they were discarded.
the pure dihydrogenphosphate salt dried very fast, was not noticably hygroscopic and was sparkling white. it was not recrystallized before...

...the bioassay of an unknown dose, maybe 15-25mg of the salt via nasal administration, confirmed the beneficial properties of said compound described in the paper available from rhodium. the onset was rapid, stimulation was gentle and there was no dilation of the pupils at all times. heart frequency was slightly increased, but never uncomfortable. as noticed with any stimulant of the phenethylamine type, there was significant vasoconstriction in the genitals (generally referred to as "chemistry cock" where the subject lives Smile

. there was also no "transition chill" as noticed with the sulfate. the plateau lasted about 3 hours, the whole experience about 4 hours. there was no apparent neurotransmitter depletion as usually strongly present upon administration of the sulfate salt. no hangover, no noticable after effects.
the administered substance would thus be referred to by swim as an ideal stimulant for therapeutic use.

there will certainly be more trials of phenethylamine phosphate salts.

it would be favorable to define conditions in which the formation of salts other than the desired dihydrogenphosphate could be excluded.

Vitriodor · Thu Jul 07, 2005 6:29 am

Lego · Thu Jul 07, 2005 1:40 pm

joe_aldehyde · huxleys associate

Vit: as described in the paper swim referenced to, the dihydrogenphosphate is a flocculent powder which is suspended in the solvent and keeps doing so upon vigorous stiring, whereas the hydrogenphosphate (probably with the inclusion of H3PO4 molecules) is a paste and settles to the bottom.
swim excluded the possibility of impurities forming any byproducts with phosphoric acid since the paste-like substance was soluble in water and yielded a precipitate upon base addition, which could be converted to the flocculent powder described earlier. swim guesses this is being called "empirical knowledge".

swim had no means of determining mp. or ambitions of doing a DC with the powder since its properties were as described and there were no major fuckups in the synthesis of the free amine, so the salt was assumed to be reasonably pure.

swim don't know of the appearance that MDMA*H3PO4 has, but his AMPH*H3PO4 is also a bit "chalk like", but unless in big chunks every powder is substiantially "chalk-like". crystals might only be obtained if recrystallized, while swim don't see any use for that since his salt was snow-white.
swim also don't see any sense in making HBr salts. you could save your precious HBr for other things.

Vitriodor · Fri Jul 08, 2005 2:04 am

Lego, Joe, thanks for clarifying. Actually, I should have known better. When looking at an acid/base constants table, for H3PO4 7.4*E-3 (mol/lit) is given, for H2PO4- it is already 6.2*E-8 and for HPO42- it is 4.8*E-13. This explains why the triple salt hardly will be formed. For sulphates on the other hand, the second proton acidity is high (1.2*E-2) and therefor disalts will form.

In relation to MDMA phoshate crystallisation, suddenly it all becomes clear to me what is happening. Next to a fine powder a paste, as Joe just described, is formed. It really sticks to the bottom/walls (and in this way you can easily separate the two as described). After filtration of the whole mixture, followed by drying and grinding, the resulting powder feels what I call "chalk like" (dusty?) in contrast to MDMA HCl powder which is more crystalline. Another difference observed: it is difficult to get a white powder when making MDMA phosphate, it always has an off-white appearance and recrystallisation (in acetone) did not improve it very much. For MDMA HCl it is not difficult to get a white crystalline material however.

About using HBr for crystallization, I actually never did that, but it is possible as I learned from another bee. Again I have to agree: I don´t see any advantage doing so.
Vit

radio879dmt · Sat Jul 09, 2005 7:42 pm

Nice! I was always interested in this.. but it sounds like the best salt to make of amphetamine for sure Smile

the alchemist · Mon Jul 11, 2005 6:31 am

How does amphetamine compare with dextro-amphetamine? Does the other isomer produce an effect?