HRID1199355
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
PROCEDURE
实验过程
Sodium borohydride (10 g) is added with stirring to a solution, boiling under reflux, of 1-methyl-4-(2,4,6-trimethoxyphenyl)-piperidin-3-one in absolute ethanol. Stirring and heating under reflux is then continued for a further hour. On cooling, the reaction mixture is diluted with water, then concentrated in order to remove the ethanol and extracted with chloroform. The chloroform extract is washed with water, dried over anhydrous sodium sulfate and concentrated to give a solid residue which, on crystallization from acetone, gives the desired product (29.2 g) of melting point 124°-125° C.
WORKUP
后处理
- stirringStirring
- temperatureheating
- temperatureunder reflux
- waitis then continued for a further hour
- temperatureOn cooling
- concentrationconcentrated in order
- customto remove the ethanol
- extractionextracted with chloroform
- extractionThe chloroform extract
- washis washed with water
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated
- customto give a solid residue which
- customon crystallization from acetone