10-10-01 20:16
No 223014
Folowing the Agent Smith OTC I gassed safrole with HBr
and now the mixture turned green. I gassed it again and
now it is a very dark green almost looks black. Is
this Bromosafrole? I heard that is should go.... green,
blue,purple, burgundy? Is this bromosafrole? Do I need to
do something else? Should I animate it now?
Im kind of stumped on this one...
Rhodium , Agent Smith... other bees? Any ideas?
Gott Mit Uns!
(Hive Bee)
10-11-01 02:32
No 223106
Did you have the Safrole in a solvent of sorts or did you just bubble the HBr through it?
You Bromosafrole will have to be distilled out of the mixture after some washing and possibly seperation from other layers (in case of two phase with GAA).
As soon as you've isolated your Bromosaf you could just dissolve it in MeOH and add MeAM in MeOH and chuck into a bomb. 130C in the bomb for 2-3 hours should be fine.
Good luck
(Newbee)
10-11-01 03:28
No 223120
hmmmmmmm did you gas it in an ice-NaCl bath? Make sure to wash it w/NaHCO3-etc. to remove any excess acid beefore proceeding w/amination.
Sweet dreamz,
IudexK
(Newbee)
10-11-01 20:16
No 223477
Ok....
I bubbled the HBr into the safrole directly. I did not
use any chloroform. If I had used the chloroform would
things have gone differnetly? Can i seperate the
bromosafrole without distilling. I REALLY want to avoid
that. I did not have the safrole in an ice bath. Should
I have the safrole in an ice bath?
What exactly does the chloroform do?
Thanks for you help!!
Gott Mit Uns!
(Hive Bee)
10-12-01 16:31
No 223827
pardon my stupidity but:
Is it possible that denatured alcohol (anhydrous 96%
ethanol, 4% methanol) could be used as a replacement
for MeOH?
If MeOH is only used as a solvent, this could be true?
(assuming anhydrous).
I've checked the search engine to no avail.
feel free to bitch.
Don't mind me. I'm mentally ill.
(Hive Bee)
10-12-01 17:00
No 223836
Yes, you must cool the safrole in an ice-NaCl bath. You should use a solvent. DMSO or DMF are ideal. I don't know if MeOH would work. If it would, denatured EtOH should work too. You can proceed with the amination directly without distilling, although yields will be lower. Try to use anhydrous HBr. Anhydrous HBr gassed thru a soln. of safrole in DMF @0C should give ~95% yields...
Sweet dreamz,
IudexK
(Hive Bee)
10-13-01 13:29
No 224092
Actually, upon looking, denatured alcohol would seem
to work. Ethanol is almost as polar as methanol, and
it is classed as a protic solvent, which is what the
reductive amination takes place in. Furthermore, it
also contains some amount (4%) of methanol in it also.
So anhydrous denatured alcohol (96% ethanol 4% methanol)
should be a perfectly fine medium for the amination to
take place.
Comments?
Don't mind me. I'm mentally ill.