11-09-04 15:15
No 540714
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...
(Hive Adickt)
11-09-04 23:57
No 540781
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.
(Hive Bee)
11-10-04 00:11
No 540783
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..