09-09-03 15:30
No 457899
Ok just thought that I would post my friends results. He was able to obtain 2CH. He used the regioselective iodination proceedure on rhodiums site. There were a few mistakes made but I think it went ok. First off he used a 250ml flat bottom flask. The stirbar that he used was too small for the bottom of the flask so he had buildup of solids around the bottom edges that was not getting stirred( he thinks it was oxone). He used 1.2g of 2CH*HCl, 1.9g of KI, and 4g of oxone. He used slightly higher amounts of KI based upon the discussion in bariums thread(I will post a link to this thread when I have time to look it up.
First off he noticed that he needed to use more methanol(substantially more) then was posted in bariums thread. The KI would not dissolve in 10ml of methanol- even after breaking up the big chunks he tried hardcore magnetic stirring, nothing would work except more. He added the chemicals in the sequence outlined in bariums writeup and the paper, added the oxone in 3 separate portions over 10 minutes and allowed it to stir for exactly 24 hours. Now he was sure that the reaction was not going to be ideal due to the too-small stirbar and the oxone that collected in the corners and did not mix for the full 24 hours.
The reaction mixture was poured into a 250ml separatory funnel and washed with 2 50ml portions of DCM. This was not a sufficient wash, it took 3 more 40-60ml DCM washes to pull all of the soluble impurities out of the mixture, the last wash yeilded a clear DCM layer, and the aqueous layer was not colorless as I expected based on Bariums writeup(my friend was of course doing this slightly different being as though he started with 2CH*HCL) but the solution was a mucky orange brown. Next NaOH was added to the mixture until the ph was brought to 12, three or four 50ml DCM extracts were done, and the DCM extracts that should contain the 2CI were a clear clean yellow color. These were combined washed with water and evaporated on pyrex dish to yeild 0.6g of a clear yellow oil, which was scraped up with a razor into a puddle, this puddle started to harden almost instantly and within minutes turned into a pile of whitish, but slightly pink hard dry powder. This same thing happened to a friend of his while doing a mescaline extract before, he was left with a clear yellow oil that crystalized into a solid white rock of powder as soon as it was scraped up.
So this is where the experiment left off. He had to go out of town that night and as soon as the stuff was bagged and put in the freezer he left. So now he is going to neutralize and recrystalize from IPA. He wondered about one thing and he should not even ask he should just do it as was reccomended in both writeups, but making a dry hcl solution of IPA, will be a bit hard. He can do it if need be, but he wondered if the more experienced bees though it would be ok to add technical grade concentrated HCL to pre-dried IPA and recrystalize? It would not be completely dry because of the water in the HCL, but this is a very small amount and he thought that maybe it would still crystalize despite the small amount of water.
If I do not get any feedback I will instruct my friend to just make the dry IPA solution and go that route. The reason he thought that just adding the concentrated HCL would work is because he recalls in Bariums post a quote from shulging saying that none of the 2C's are "particularly soluble" in water accept 2CH. So he thinks that it may be ok with a bit of water, and it may even make it harder for the leftover 2CH to crystalize with the final product.
My friend is pretty sure that he has 2CI in that .6g bag, he will post results after he completes the recrystalization.
Later
ApoStLe oF cHaoS
(I'm Yust a Typo)
09-09-03 18:40
No 457922
A few drops of technical grade HCl (37%) added to some freebase in IPA will do just fine. The water from the HCl doesn't hurt. You might try adding some ether to the mix to loosen it up.
(Stranger)
09-16-03 23:35
No 459455
Your friend might want to consider using 2c-h freebase aswell instead of 2c-h hcl, using 2c-h hcl it might give a mix of 2c-c and 2c-i.
Hippler