10-28-03 23:27
No 467467
SWIM weighed out 14.4g 2CH freebase dissolved it in 14.4g Glacial Acetic Acid in Flask 1. In Flask 2 SWIM weighed out 14.4g Br2 and added it to 14.4g Glacial Acetic Acid. Flask 2 was then poured into Flask 1. After 30 min, SWIM looked at SWIMs reaction which has much 2CB extra red/brown from Bromine sorta slushy consistency. This is SWIM's first 2CB rxn attempt. SWIM plans on cleaning up the excess Br2 from the 2CB HBr by washing the 2CB/Bromine/GAA slush w/ chilled Glacial Acetic Acid in a Buchner Funnel and then recrystallize the 2CB HBr filtrate with boiling IPA. How does this sound to you more knowledagble and experienced bees? Thanks in Advance!!
'A Helpful Bee, is a Friend Indeed'
(Newbee)
10-29-03 10:49
No 467597
Washing the crystals with the GAA and recrystallisation using IPA should work fine, prior to recrystallisation you might want to wash of the last bit of acetic acid using ether.
Also you might want to try and learn something about molar calculations the next time you do a reaction instead of using equal ammounts of bromine and 2c-h
for example in the formation of 2c-b hbr , 2c-h and br2 are reacted in equimolar ammounts.
so if you want to react 14,4 gram of 2c-h you would need aproximateley 12,69834368 grams of br2 :
181.234 grams 2c-h/mol
159.808 gram br2/mol
14.4 / 181.234 = 0,07946 mol 2c-h
0,07946 mol br2 * 159,808 = 12,69834368 grams of br2
Hippler
(Chief Bee)
10-29-03 14:52
No 467667
Take a look here for a detailed procedure: ../rhodium /2cb.bro