反应详情

Sodium (3.6 g) was added by portions to ethanol (92 ml) over 2 hours, while the solution was stirred at room temperature. Thereafter, ethyl acetoacetate (10 ml) and acetamidine hydrochloride (7.42 g) were added to the reaction solution, and the obtained mixture was stirred at 70° C. for 16 hours. Thereafter, the reaction mixture was stirred at 100° C. for 9 hours, and the temperature of the reaction solution was returned to room temperature. Concentrated hydrochloric acid was added to the reaction solution, so that the pH value was adjusted to around 5. The obtained mixture was concentrated under reduced pressure, so as to obtain a crude title compound (25.6 g).

1. stirringthe obtained mixture was stirred at 70° C. for 16 hours
2. stirringThereafter, the reaction mixture was stirred at 100° C. for 9 hours
3. customwas returned to room temperature
4. concentrationThe obtained mixture was concentrated under reduced pressure