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All 10 posts Subject: 2CH Bromination Please login to post Down

kjb1891
(Stranger)
03-08-04 04:08
No 493691
      2CH Bromination

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
(Hive Bee)
03-08-04 04:18
No 493694
      ask the inventor

click on the PIHKAL link on the bottom of the page, then click on 2C-B.

wolfx
(Hive Bee)
03-08-04 16:54
No 493766
User Picture       Bromine

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
(Chief Bee)
03-08-04 18:59
No 493783
User Picture       Prep of 2C-B.HBr

https://www.rhodium.ws/chemistry/2cb.bromination.html

^{The Hive - Clandestine Chemists Without Borders}

kjb1891
(Stranger)
03-08-04 19:26
No 493788
      Chilling the bromine would help reduce the...

Chilling the bromine would help reduce the evaporation wouldn't it?

Rhodium
(Chief Bee)
03-08-04 19:32
No 493789
User Picture       Yes, that is also covered in the document I...

Yes, that is also covered in the document I linked.

^{The Hive - Clandestine Chemists Without Borders}

kjb1891
(Stranger)
03-08-04 21:40
No 493804
      Would the acetic acid and ethyl acetate be...

Would the acetic acid and ethyl acetate be sufficient enough for getting rid of impurities? Thanks for all the info

Vaaguh
(Hive Bee)
03-09-04 14:09
No 493946
      getting rid of the impurities

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.

Hippler

kjb1891
(Stranger)
03-10-04 19:54
No 494245
      I meant to say washing with the acetic acid,...

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
(Hive Bee)
03-11-04 10:44
No 494362
      cleanup

A suggestion might bee washing with ethyl acetate followed by cold dry ether and for the recrystalisation either ether/methanol or ether/ipa.

Hippler

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	All 10 posts		Subject: 2CH Bromination		Please login to post		Down


		kjb1891 (Stranger) 03-08-04 04:08 No 493691				2CH Bromination
						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 (Hive Bee) 03-08-04 04:18 No 493694				ask the inventor
						click on the PIHKAL link on the bottom of the page, then click on 2C-B.



		wolfx (Hive Bee) 03-08-04 16:54 No 493766				Bromine
						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 (Chief Bee) 03-08-04 18:59 No 493783				Prep of 2C-B.HBr
						https://www.rhodium.ws/chemistry/2cb.bromination.html ^{The Hive - Clandestine Chemists Without Borders}



		kjb1891 (Stranger) 03-08-04 19:26 No 493788				Chilling the bromine would help reduce the...
						Chilling the bromine would help reduce the evaporation wouldn't it?



		Rhodium (Chief Bee) 03-08-04 19:32 No 493789				Yes, that is also covered in the document I...
						Yes, that is also covered in the document I linked. ^{The Hive - Clandestine Chemists Without Borders}



		kjb1891 (Stranger) 03-08-04 21:40 No 493804				Would the acetic acid and ethyl acetate be...
						Would the acetic acid and ethyl acetate be sufficient enough for getting rid of impurities? Thanks for all the info



		Vaaguh (Hive Bee) 03-09-04 14:09 No 493946				getting rid of the impurities
						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. Hippler



		kjb1891 (Stranger) 03-10-04 19:54 No 494245				I meant to say washing with the acetic acid,...
						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 (Hive Bee) 03-11-04 10:44 No 494362				cleanup
						A suggestion might bee washing with ethyl acetate followed by cold dry ether and for the recrystalisation either ether/methanol or ether/ipa. Hippler

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