purification of 4-bromo-2,5-dimethoxyphenethylamine?

auttie · Fri Jun 03, 2005 8:20 am

any known methods for washing excess bromine from 4-bromo-2,5-dimethoxyphenethylamine Hydrobromide besides ethyl acetate and ether? preferably one that uses OTC chems and doesnt need to vaccum distil the freebase(but please list any known ways). and would thoose also be good to clean 4-bromo-2,5-dimethoxyphenethylamine hydrochloride? can you clean the hydrochloride with ethyl acetate and ether?

~thanks

anime · Fri Jun 03, 2005 8:53 am

bromine dissolves in DCM, DCM as your know is OTC (paint stripper).

loki · guinea pig

i'd say tolly would work too, as would naptha... certainly, these solvents pull out iodine anyway.

auttie · Sun Jun 05, 2005 9:58 pm

well the hardware store was closed.. so first swim tried xyline.. which proved completely worthless and made the flat stink for a bit. After sitting around for a bit.. swim decided to check out the solvent solubility chart.. where swim saw isoalchihol and THF.. wallaa.. Swim had the thf from his run in with lah a few months back.. swim pored a bit of the thf into a beaker with the 4-bromo-2,5-dimethoxyphenethylamine, let sit for 10 min.. and then ran the solution thru the vacuum filter for 15 min.. repeated 3 times. It is beleived that swim lost a bit of the honey(prolly close to 1/8.) in this washing technique however the thf allowed him to get whitest crystals he has seen thus far (used ethyl acetate last time). this works on both the hbr and the hcl. better documentation will be done on the washing next time =].

stoopid1980 · Tue Jun 07, 2005 11:37 am

I've heard of cold acetic acid being used to wash the excess Br out. I've also heard that the 2C-B can degrade far more rapidly if the Br isn't washed out so clean 'er up. 30 mg of HBr is about equivalent to 25 mg Hcl. Hope this helps.

auttie · Wed Jun 08, 2005 12:04 am

degrade how? the HCL is very very clean, but the HBR still has a vinagery smell... should I be worried about a loss of potency with the HBR?

stoopid1980 · Thu Jun 09, 2005 9:23 am

I would go with cold acetic acid washes if it still has that odor. That's my opinion though. If washed again and stored properly I don't think you'll see much degradation. I didn't. Mine hasn't lost any potency, though. I love the 2C-Beeees.

Ionium · Wed Aug 17, 2005 2:56 am

Cold GAA washes followed by ether washes, and then 2-3 recrystallizations from boiling IPA. This will work for the HBr-salt, probably not for the HCl-salt.

Stinging_Nettle · Wed Aug 17, 2005 11:57 am

You can just use acetone in my humble opinion to 'wash' the crystals.

icecool · Insistent Chemist

Well not for the hydrobromide salt, it dissolve quite well in acetone.

icecool · Insistent Chemist

So for recrystalizing 2C-B.HCl would it be a good idea too warm up ether and dissolve the crystals in there.
And then put let it cool down again and then eventually let it cool to -18*C and then filtration?
And also some washing with ice-cold GAA...

the alchemist · Thu Aug 18, 2005 7:13 pm

Disolve 2CB•HCl in minimum amount of boiling IPA, let cool to >35° C (so Et2O does not boil off). Dilute with some Et2O until turbidity persits but eventually disappears with vigorous stirring and/or heating. Cover and let cool to room temp. If no crystals form overnight, refrigerate.

Radiumhero · Thu Aug 18, 2005 10:56 pm

yea do 2 recristalliastion from pref ipa if not avaialble ( should be )
try buOH , and giv it some nice light perhaps from an projector or else
this will help the reactive bromine to substitute th H groups of the alkohol
and ur freed of the nasty shit ...