HRID1199355

反应详情

EQUATION

反应方程式

HRID 1199355 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. stirringStirring
  2. temperatureheating
  3. temperatureunder reflux
  4. waitis then continued for a further hour
  5. temperatureOn cooling
  6. concentrationconcentrated in order
  7. customto remove the ethanol
  8. extractionextracted with chloroform
  9. extractionThe chloroform extract
  10. washis washed with water
  11. dry with materialdried over anhydrous sodium sulfate
  12. concentrationconcentrated
  13. customto give a solid residue which
  14. customon crystallization from acetone