Author Topic: ammonium chloride-> MDA  (Read 1435 times)

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entin88

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ammonium chloride-> MDA
« on: July 20, 2003, 07:06:00 PM »
Is this correct that you can sub. ammonium chloride for methylamine and produce MDA. I used the search enine but did not find any good ref. for this.
The reason I used this approach is that I was totally unable to make the methylamine hydrochloride (methylammonium chloride, MA.HCl) by any method. I tried BrightStar's method, as well as about 4 other methods I found on the web. In all cases, I was able to make what were probably mixtures of MA.HCl and ammonium chloride, but I couldn't figure out how to assess the purity. I also didn't have any luck getting the stuff I needed to do a purification: absolute ethanol is difficult to obtain; in California, the best you can purchase at a liquor store is about 75%, so you're faced with a distillation even to get to 95%. Then you've got to get some anhydrous calcuim oxide, and I didn't know how to do that. I even made a bunch of chloroform to clean out other impurities (which you should do), and that was a pain in the butt and perhaps a bit dangerous, too.

The problem is that the ammonium chloride will cheerfully react by the same mechanism as the MA.HCl with the MDP-2-P, but it will make MDA in place of MDMA. I would not have minded a mixture of, say, 3% MDA and 97% MDMA, but I just didn't know what I'd get. Anyway, the method described below worked perfectly, and should make exactly 0% MDA and 100% MDMA.

Rhodium

  • Guest
purifying methylamine.hcl
« Reply #1 on: July 20, 2003, 08:06:00 PM »
You can recrystallize the methylamine from isopropanol if you don't have ethanol (but it is a little bit too soluble in  methanol for my taste). Ammonium chloride is very sparingly soluble in isopropanol, so it is easy to filter off when the methylamine.HCl has dissolved.

Also, if you have a 90:10 mixture of MeNH2.HCl/NH4Cl and use that to aminate MDP2P, you'll get 99:1 MDMA:MDA anyway, as methylamine is so much more reactive (and if you recrystallize that product, you will get practically pure MDMA).

Even if you use only NH4Cl and try to aminate MDP2P with that, you'll only get 20-30% yield of MDA as NH4Cl adds so badly to MDP2P...

terbium

  • Guest
Stepwise evaporaton
« Reply #2 on: July 20, 2003, 11:16:00 PM »
but I couldn't figure out how to assess the purity. I also didn't have any luck getting the stuff I needed to do a purification: absolute ethanol is difficult to obtain; in California, the best you can purchase at a liquor store is about 75%, so you're faced with a distillation even to get to 95%. Then you've got to get some anhydrous calcuim oxide, and I didn't know how to do that. I even made a bunch of chloroform to clean out other impurities (which you should do), and that was a pain in the butt and perhaps a bit dangerous, too.
If you had read my extensive posts on the subject you  would know that if you follow the stepwise evaporation and crystallization procedure as per Vogel then neither the alcohol recrystallization or chloroform wash is necessary to obtain reasonably pure methylamine. You can get a half way decent idea of the purity by appearance - ammonium chloride is short needle like crystals while methylamine hydrochloride is large snowflakes. For additional purity without recrystallization you can also use partial neutralization of an aqueous ammonium chloride/methylamine hydrochloride solution which preferentially drives off ammonia and has also been discussed here. If you want quantitative knowledge of the amount of ammonia in your methylamine you can titrate and follow the titration with a pH meter, a procedure which I have also discussed here.