HRID225703

反应详情

EQUATION

反应方程式

HRID 225703 的结构方程式

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A mixture of 4.26 mmol 2-chloro-5-methanesulfonyl-benzoic acid (Example B1(a)) in 8 ml morpholine was heated at 110° C. for 15 h. After evaporation of all volatiles the residue was acidified by addition of 1 N HCl and extracted three times with ethyl acetate. The combined organic extracts were washed sequentially with 1 N HCl and saturated brine, dried over sodium sulphate, and concentrated in vacuo to afford the title compound as a light yellow amorphous solid (58%). MS (m/e): 284.1 ([M−H]−, 100%).

WORKUP

后处理

  1. customAfter evaporation of all volatiles the residue
  2. additionwas acidified by addition of 1 N HCl
  3. extractionextracted three times with ethyl acetate
  4. washThe combined organic extracts were washed sequentially with 1 N HCl and saturated brine
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated in vacuo