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Amt-nitrostyrene?

Started by Grignard, November 09, 2004, 03:15:00 PM

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Grignard

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

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

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..