HRID1461655

反应详情

EQUATION

反应方程式

HRID 1461655 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

34.4 g (0.1 mol) of N-(3-chloro-α,α-dimethylbenzyl)-N-(2-oxopropyl)phenylacetamide prepared in accordance with the method of Reference Example 6, was dissolved in 200 ml of ethanol, and 0.5 (0.009 mol) of sodium hydroxide powder was added thereto. The mixture was refluxed under heating for 10 minutes. Then, the solvent was distilled off under reduced pressure, and then water was added thereto. The mixture was extracted with ethyl acetate. The ethyl acetate layer was dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure, followed by purification by silica gel column chromatography (n-hexane/ethyl acetate) to obtain 21.2 g (yield: 65.2%) of the desired compound.

WORKUP

后处理

  1. temperatureThe mixture was refluxed
  2. temperatureunder heating for 10 minutes
  3. distillationThen, the solvent was distilled off under reduced pressure
  4. additionwater was added
  5. extractionThe mixture was extracted with ethyl acetate
  6. dry with materialThe ethyl acetate layer was dried over anhydrous magnesium sulfate
  7. distillationthe solvent was distilled off under reduced pressure
  8. customfollowed by purification by silica gel column chromatography (n-hexane/ethyl acetate)