反应详情

温度

40 °C

Acetamidine hydrochloride (3 mol) and 4-dimethylamino-1,1-dimethoxy-but-3-en-2-one (2 mol) were mixed in methanol (500 ml) and the reaction mixture was warmed to 40° C. A solution of sodium methoxide in methanol (558 g, 30%) was added quickly and a brown suspension was formed. The reaction mixture was heated under reflux for 2 h, cooled to room temperature overnight followed by evaporation of methanol under reduced pressure. The resulting residue was taken up in dichloromethane (500 ml) and washed several times with water (100 mL). The solvent was removed to give 307 g of black oil. The distillation of this oil gave a colourless liquid of boiling point 55-58° C. (0.5 mbar).

1. customa brown suspension was formed
2. temperatureThe reaction mixture was heated
3. temperatureunder reflux for 2 h
4. temperaturecooled to room temperature overnight
5. customfollowed by evaporation of methanol under reduced pressure
6. washwashed several times with water (100 mL)
7. customThe solvent was removed