HRID2263939

反应详情

EQUATION

反应方程式

HRID 2263939 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 5-chlorosulfonyl-2-ethoxy-4-methoxybenzoic acid (13 g, 44 mmol) in tetrahydrofuran was cooled to 5° C. and treated with excess diazomethane in ether solution (prepared from N-methyl-N-nitroso-p-toluenesulfonamide, Aldrich) and stirred for 10 min. Solvent and excess diazomethane was removed by rotary evaporation. The resulting residue was dissolved in dichloromethane and filtered through a plug of silica gel and evaporated. The solids were triturated with ether/hexane to give 13 g of 5-chlorosulfonyl-2-ethoxy-4-methoxy-benzoic acid methyl ester as a colorless solid.

WORKUP

后处理

  1. customSolvent and excess diazomethane was removed by rotary evaporation
  2. dissolutionThe resulting residue was dissolved in dichloromethane
  3. filtrationfiltered through a plug of silica gel
  4. customevaporated
  5. customThe solids were triturated with ether/hexane