Author Topic: Amt-nitrostyrene?  (Read 2395 times)

0 Members and 1 Guest are viewing this topic.

Grignard

  • Guest
Amt-nitrostyrene?
« on: November 09, 2004, 03:15:00 PM »
I condensated indole-3-carboxaldehyde with nitroethane as in the ultrasound promoted nitrostyrene dokument at rodiums page.. i tested the reaction mix on tlc after 3 h but i got a lot of aldehyde left and let the mix stand over night.. when i came next morning there was a lot of small yellow crystalls in the bottom of the round bottom and the aldehyde was almost gone (by tlc), so i evaporated the solvent and try to rextallize from boiling MeOH.. but the yellow crystaline mass do not solved. And when i put it in the fridge a lot of needle like brown crystalls start to form.. what could this yellow crystalls be and is the styrene from this compound brown needels? should i filter the yellow mass from the hot MeOH and proceed to the next step with the brown crystalls? diffused?? yes... :P  :P

hest

  • Guest
Xtals
« Reply #1 on: November 09, 2004, 11:57:00 PM »
Overnight with UltraSound  ???
The typical polutant is the dimer, and that's a dead end.
disolve the material in app 10mL MeOH/g decant the MeOH from the brown stuff and put the MeOH in the fridge.

Ant next tim follow your reation home, dont let them sit.

Grignard

  • Guest
so the ultrasound has destroyed some of the...
« Reply #2 on: November 10, 2004, 12:11:00 AM »
so the ultrasound has destroyed some of the material? But this synt vasn`t any good for this aldehyde, because the aldehyde remains unsolved in the nitroethane throgh the sonication.. aldehyde was purchased from a lab company.. So all the yelow stuff must be filtered from the meOH and i will proceed with the crystalls that solved in hot MeOH.. I followed the procedure just as it stands on rhodium..