反应详情

温度

85 °C

To a solution of 50 mL ethanol and 15 mL conc. hydrochloric acid was added 4.35 g (0.014 mol) of the product of Step A and the reaction mixture was stirred and heated to 85° C. using an external oil bath for 3 h. The reaction mixture was then cooled to room temperature and evaporated in vacuo. Excess water was removed from the product mixture by azeotropic distillation of added portions of toluene on a rotary evaporator. The residue was triturated with ether and dried overnight in vacuo to afford the title compound as a white crystalline solid.

1. customfor 3 h
2. temperatureThe reaction mixture was then cooled to room temperature
3. customevaporated in vacuo
4. customExcess water was removed from the product mixture by azeotropic distillation of added portions of toluene on a rotary evaporator
5. customThe residue was triturated with ether
6. customdried overnight in vacuo