反应详情

温度

120 °C

A mixture of ethyl acetoacetate (1.5 g, 11.5 mmol) and dimethylformamide dimethyl acetal (1.68 mL, 12.7 mmol) was stirred at 120° C. for 2 hours. The reaction solution was cooled to room temperature, and a solution of phenyl hydrazine hydrochloride (1.67 g, 11.5 mmol) in ethanol (30 mL) was then added thereto. The obtained mixture was stirred at 80° C. for 2.5 hours. The reaction solution was cooled to room temperature, and it was then concentrated under reduced pressure. The residue was purified with a fractionation purification apparatus (Biotage, ethyl acetate:hexane=1:19-3:7), so as to obtain the title compound (2.32 g, 87%) in the form of a yellow oily product.

1. temperatureThe reaction solution was cooled to room temperature
2. stirringThe obtained mixture was stirred at 80° C. for 2.5 hours
3. temperatureThe reaction solution was cooled to room temperature
4. concentrationit was then concentrated under reduced pressure
5. customThe residue was purified with a fractionation purification apparatus (Biotage, ethyl acetate:hexane=1:19-3:7)