反应详情

10.7 g of 2,3-dichlorophenacylamine hydrochloride and 6 g of methyl 3-dimethylaminoacrylate are heated for 2 hours under reflux in 120 ml of ethanol. Then a solution of 4 g of sodium ethylate in 40 ml of ethanol is added dropwise and the reaction mixture is heated for another hour under reflux. The reaction mixture is then concentrated by evaporation and the oily residue is purified by column chromatography (silica gel; elution with a 3:1 mixture of toluene/ethyl acetate. Melting point: 205°-206° C.

1. temperaturethe reaction mixture is heated for another hour
2. temperatureunder reflux
3. concentrationThe reaction mixture is then concentrated by evaporation
4. customthe oily residue is purified by column chromatography (silica gel
5. washelution
6. additionwith a 3:1 mixture of toluene/ethyl acetate