反应详情

A solution of 13.4 g of 95% potassium tert-butylate in 72 ml of ethanol is added over 6 minutes to a solution, stirred and heated to 50° C., of 18 g of 2,6-dimethoxyacetophenone in 54 ml of ethanol. The mixture is heated to reflux, 16.3 ml of ethyl oxalate are added over 9 minutes and refluxing is continued for 1 hour. 40 ml of ethanol are then distilled off and the mixture is allowed to cool with stirring for two and a half hours. The mixture is filtered, and the precipitate is washed with 40 ml of ethanol and dried under vacuum at 60° C. for 17 hours to obtain 31 g of expected product.

1. temperatureThe mixture is heated
2. temperatureto reflux
3. temperaturerefluxing
4. distillation40 ml of ethanol are then distilled off
5. temperatureto cool
6. stirringwith stirring for two and a half hours
7. filtrationThe mixture is filtered
8. washthe precipitate is washed with 40 ml of ethanol
9. customdried under vacuum at 60° C. for 17 hours