Oxygen69 (Stranger)
08-11-03 01:54
No 452848
      Bromination of 2C-H HCl  Bookmark   

What are the disadvantages of brominating 2C-H HCl rather than 2C-H freebase?  I understand that equimolar amounts of Br2 are to be used in either case, and that use of the salt will result in the creation of HBr.  This means that the reaction must be done with adequate ventilation.  Could the HBr somehow attack the product, reducing yields and/or purity?  What would happen if someone added an equimolar amount of sodium acetate with the 2C-H HCl?

Also, does the reaction need to be done with magnetic stirring?  I am under the impression that it could be done in a coffee cup stirred by a glass rod.

One more thing - Wouldn't it be better to recrystalize the product from boiling IPA/DCM rather than purifying via Shulgin's method?  It is interesting to note that Shulgin's HBr salt has a narrower melting point range than his HCl salt, and that others have mentioned problems with 2C-B HCl hydrates.  Perhaps he forms the HCl salt for reasons other than what he suggests?

Oxygen69
 
 
 
 
    Vitus_Verdegast
(Hive Bee)
08-11-03 02:56
No 452853
      LOL!!  Bookmark   



Also, does the reaction need to be done with magnetic stirring?  I am under the impression that it could be done in a coffee cup stirred by a glass rod.




laughlaughshockedcrazy
At least buy a pyrex (or any heat-proof lab-) beaker!

Also a mag stirring device is not hard to make yourself, eg. from an old disk driver. UTFSE.


A Dream Within A Dream (http://www.poedecoder.com/Qrisse/works/dreamw.html)
 
 
 
 
    Oxygen69
(Stranger)
08-11-03 06:13
No 452908
      Well, of course!  Bookmark   

heh.  I wouldn't actually perform this reaction in a coffee cup.  I was merely pointing out how easy the reaction is to perform.  I can easily get a real magnetic stirrer.
 
 
 
 
    Oxygen69
(Stranger)
08-11-03 09:53
No 452936
      Addendum  Bookmark   

I should mention that the reaction that I'm referring to is Shulgin's bromination of 2C-H freebase, substituting equimolar amounts of 2C-H HCl and sodium acetate for 2C-H freebase.  I believe that this would result in the production of 2C-B HBr without producing nasty HBr gas.  Can anyone confirm this?  Is this a stupid idea?
 
 
 
 
    Rhodium
(Chief Bee)
08-12-03 17:55
No 453119
      The salt is all right, the glass rod is not.  Bookmark   

You need to have good magnetic stirring. You will not achive the stirring capabilities needed for a homogenous reaction with a glass rod.

Your proposal will work as long as you use enough solvent to get a clear solution before adding the bromine. But on the other hand, not much HBr gas is evolved when doing the reaction the Shulgin way, it is enough to cover the beaker with some Al foil.

Also note Post 453115 (Rhodium: "2C-B salts", Methods Discourse)