HRID1526246
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 90 °C
PROCEDURE
实验过程
To a mixture of 1-methyl-4-[1-(4-nitrophenyl)piperidin-4-yl]piperazine (4.84 g) and 1,2-dichloroethane (50 mL) was added 1-chloroethyl chloroformate (2.2 mL), followed by stirring at 90° C. for 3 hours. The solvent was evaporated under reduced pressure and then methanol (85 mL) was added thereto, followed by heating and refluxing for 1 hour. The solvent was evaporated under reduced pressure and the obtained residue was washed with ethyl acetate to obtain 1-[1-(4-nitrophenyl)piperidin-4-yl]piperazine monohydrochloride (3.74 g) as a yellow solid.
WORKUP
后处理
- customThe solvent was evaporated under reduced pressure
- additionmethanol (85 mL) was added
- temperatureby heating
- temperaturerefluxing for 1 hour
- customThe solvent was evaporated under reduced pressure
- washthe obtained residue was washed with ethyl acetate