Author Topic: a-pyrrolidine-propiophenone - can't filter it!  (Read 1512 times)

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josef_k

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a-pyrrolidine-propiophenone - can't filter it!
« on: July 15, 2003, 07:55:00 PM »
Yesterday I first brominated propiophenon with Cu(II)Br in ethyl acetate, and then filter off the Cu(I)Br. I though that the lacrymatory effect wouldn't be felt when the brominated ketone was dissolved in a solvent, but boy was I wrong... My eyes hurt like hell, and I felt it in my troat and nose too. And it lingered on for hours also! Then I reacted the filtrate with pyrrolidine. At the end of the reflux I had a almost black solution (caused by using a rubber stopper to attach a condenser to the flask I think), so I did a sort of A/B.

First I acidified it to PH 3 with HCl. That formed two layers, but I added some "chemically pure gasoline" anyway (n-heptane?) and shaked. Then the water layer was separated and made basic. The slighly red oil layer was separeted. (I guess I should have extracted this but I didn't). I boiled this to remove any solvent. After that it was dissolved in isopropanol and I started dripping in sulfuric acid. Immidiately a white precipitate started forming (whoho! I thought..), and soon enough the whole solution was so white that you couldn't look through it. That's when I decided to filter it  and continue dripping in more acid later, to prevent any over acidification. But the problem is that the solution is completely impossible to filter. It stuffs up my filter immidiately.

After the failed filtering attempt I tasted some of the powder that stuck to the filter, and it seemed to taste slightly salty at some parts, and bitter at others. It seems that my product it contaminated with something that is so finely powdered that it clogs the filter. A salt of pyrrolidine? NaSO4?

I tried to filter it through a bed of sand, like I read somewhere, but that didn't work.

What can I do so I can filter this mess? I'm not exactly experienced with any synthesis at all, so I've never had this happened to me before. It kills me to be so near, and still not there!

Btw, some time ago it was mentioned that NaBr and KBr acted sedating. Could the Cu(I)Br act in the same way perhaps? If I finaly get my product I could probably use it...

lugh

  • Guest
Celite
« Reply #1 on: July 16, 2003, 01:31:00 AM »

Post 433997

(Rhodium: "breaking up emulsions with celite", Newbee Forum)
 ;)




Barium

  • Guest
Go back a few steps
« Reply #2 on: July 16, 2003, 10:54:00 AM »
It will be easier in my opinion. Add enough water to dissolve all white crystals in the IPA then distill away all IPA. Now make the aqueous solution alkaline, saturate the solution with NaCl and extract the oil with heptane, DCM or whatever you have accessable and distill again. Why distill again you may ask.. This time you want to remove the excess pyrrolidine you have dissolved with the alpha-pyrrolidinopropiophenone. Pyrrolidine will distill at 86-88°C at atmospheric pressure. The remaining oil, which should be slightly yellow (even better if it's colorless), is now dissolved in IPA and crystallized with your acid of choice. Alpha-pyrrolidinopropiophenone hydrochloride or sulphate which is impure will become brownish-red within a day or two while the pure salt remain white.


Aurelius

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Barium
« Reply #3 on: July 16, 2003, 04:09:00 PM »
Don't forget to mention a recrystallization step after those you've listed.


Barium

  • Guest
Yes of course
« Reply #4 on: July 17, 2003, 11:37:00 AM »
Recrystalize from IPA.


Rhodium

  • Guest
Bromide as a sedative
« Reply #5 on: July 19, 2003, 03:32:00 AM »
Btw, some time ago it was mentioned that NaBr and KBr acted sedating. Could the Cu(I)Br act in the same way perhaps?

Probably not. The bromide ion is sedative at 1-2 grams, but CuBr contains only ~55% Br-, while NaBr contains ~80% Br-. Cu(I)Br is also pretty insoluble in water, and is hence not taken up very good.

josef_k

  • Guest
Filtering
« Reply #6 on: July 23, 2003, 10:19:00 PM »
Well, I went out and got myself a büchner funnel and some quality filter papers, instead of the coffee filters + coffee funnel I was using. Then when I vacuumfiltered it I got the white powder finaly.

The problem is that the powder tastes pretty salty, with just a little bitter aftertaste. And it give me no effect even with 250mg++. I'm puzzled. I don't see how it could be sodium sulfate or something like that. If you basify a solution and an oil layer separates out there shouldn't be any NaOH in the oil layer which could form sodium sulfate?

I though I had made some mistake somewhere so I basified the  "chemically pure gasoline" extract I made of the acified solution in the beginning, and that also produced an oil layer. When crystallized it produced the same slightly salty powder... God damn it.

Could it really be that a-pyrrolidinepropiophenone is so weak that you don't feel it at 250mg? Maybe I should note that I've taken my fair share of amphetamine, so I might have some tolerance, although I've not used any in over 2 months.

Kinetic

  • Guest
Yes
« Reply #7 on: July 25, 2003, 05:13:00 PM »
I made some myself a few weeks back on the recommendation of two bees, giving large variations in dose; some 25-30mg for one ;)  and the other in the hundreds of mg.

I ended up taking around 500mg, beginning with 60mg, and I too experienced pretty much no effect. No pleasant effect, that is, because at that dose my vision was absolutely screwed and I was sweating, and generally feeling pretty ill. :(  I was going to post the synthesis since it's such an easy and high yielding one, but didn't because my experience was so unpleasant. A shame, because for some reason I decided to perform the reaction on a 250mmol scale, leaving me with some 40g product still sitting in a flask...

One upside to all this was it was incredible easy to snort - no pain whatsoever. :)  This compound seems to have great differences in effects in different people; I wouldn't take it again, yet there are others who love the stuff! If you've purified it properly, maybe you could try giving some to your friends (with a suitable warning of course) to see whether they enjoy it or not.