HRID65206

反应详情

EQUATION

反应方程式

HRID 65206 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A mixture of 2.6 g of 5-(5-chlorovaleryl)-2-methoxy-benzenesulfonamide, 1.8 g of 1-(2-methoxyphenyl)piperazine, 1 g of sodium carbonate and 20 ml of dimethyl sulfoxide was stirred at 90° C. for 3 hours. After the reaction was finished, water was added to the reaction mixture and then the mixture was extracted with ethyl acetate. The extract was washed with water saturated with sodium chloride and dried over anhydrous sodium sulfate. The solvent was distilled away and the residue was dissolved in acetone followed by adding concentrated hydrochloric acid in required amount to produce crystals. The thus-produced crystals were recrystallized from methanol to obtain 2.8 g of the titled compound (yield: 61%).

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with water saturated with sodium chloride
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationThe solvent was distilled away
  5. dissolutionthe residue was dissolved in acetone
  6. additionby adding concentrated hydrochloric acid in required amount
  7. customto produce crystals
  8. customThe thus-produced crystals were recrystallized from methanol