HRID414685

反应详情

EQUATION

反应方程式

HRID 414685 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into a solution of 2 g of 7-hydroxy-4-methyl-1-indanone in 10 ml of dichloroethane was added 2.27 g of 1-piperidine sulfonyl chloride. Then 10 g of anhydrous aluminum chloride was gradually added to the mixture and stirred, and the reaction mixture was refluxed by heating for 8 hours. The reaction mixture was extracted with 200 ml of chloroform, washed with water, then the chloroform was removed by evaporation under a reduced pressure. The residue was purified by means of a silica gel column chromatography (eluent: chloroform), and recrystallized from ethanol to obtain 1.24 g of 7-hydroxy-4-methyl-6-(1-piperidinesulfonyl)-1-indanone.

WORKUP

后处理

  1. temperaturethe reaction mixture was refluxed
  2. temperatureby heating for 8 hours
  3. extractionThe reaction mixture was extracted with 200 ml of chloroform
  4. washwashed with water
  5. customthe chloroform was removed by evaporation under a reduced pressure
  6. customThe residue was purified by means of a silica gel column chromatography (eluent: chloroform)
  7. customrecrystallized from ethanol