HRID2263943

反应详情

EQUATION

反应方程式

HRID 2263943 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 4-chloro-2-ethoxy-5-methanesulfonylbenzoic acid (2.5 g, 9.0 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 4-chloro-2-ethoxy-5-methanesulfonyl-benzoic acid methyl ester (2.1 g, colorless solids).

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