Author Topic: 2CH Bromination  (Read 3552 times)

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kjb1891

  • Guest
2CH Bromination
« on: March 07, 2004, 08:08:00 PM »
So, SWIM has questions about doing bromination of 2,5-dimethoxy-PEA HCl into 2CB HBr. All you have to do is bring a solution of 2CH and GAA to a good stir. Then, add a solution of elemental bromine and GAA. Once it forms a brown crystaline mass and returned to room temps it can be cleaned up with acetic acid and ethyl acetate to give fairly good 2CB HBr. Is there anything else to it?

gsus

  • Guest
ask the inventor
« Reply #1 on: March 07, 2004, 08:18:00 PM »
click on the PIHKAL link on the bottom of the page, then click on 2C-B.

wolfx

  • Guest
Bromine
« Reply #2 on: March 08, 2004, 08:54:00 AM »
Just in case, you will need a fume hood or something like that, because of the very iritating and toxic bromine fumes.

Also, transfering the bromine with a pipette is difficult because it vaporizes and falls from the pippete.

There are alternative bromination procedures whithout using bromine. I have never tried any nor the bromine either, though. There is also a lot of posts, use TFSE.

Rhodium

  • Guest

kjb1891

  • Guest
Chilling the bromine would help reduce the...
« Reply #4 on: March 08, 2004, 11:26:00 AM »
Chilling the bromine would help reduce the evaporation wouldn't it?

Rhodium

  • Guest
Yes, that is also covered in the document I...
« Reply #5 on: March 08, 2004, 11:32:00 AM »
Yes, that is also covered in the document I linked.


kjb1891

  • Guest
Would the acetic acid and ethyl acetate be...
« Reply #6 on: March 08, 2004, 01:40:00 PM »
Would the acetic acid and ethyl acetate be sufficient enough for getting rid of impurities? Thanks for all the info

Vaaguh

  • Guest
getting rid of the impurities
« Reply #7 on: March 09, 2004, 06:09:00 AM »
No this will not get rid of all the impurities, washing the compound afterwards with cold dry ether followed by a recrystallisation will remove most impurities.


kjb1891

  • Guest
I meant to say washing with the acetic acid,...
« Reply #8 on: March 10, 2004, 11:54:00 AM »
I meant to say washing with the acetic acid, but doing a recrystallization with the ethyl acetate as the solvent. Or is there a better solvent to use?

Vaaguh

  • Guest
cleanup
« Reply #9 on: March 11, 2004, 02:44:00 AM »
A suggestion might bee washing with ethyl acetate followed by cold dry ether and for the recrystalisation eitherĀ  ether/methanol or ether/ipa.