HRID1930995

反应详情

EQUATION

反应方程式

HRID 1930995 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

To 4.1 mmol 2-hydroxy-5-methylsulfamoyl-benzoic acid methyl ester and 4.1 mmol potassium carbonate in 5 ml DMF was added dropwise 6.1 mmol trifluoro-methanesulfonic acid 2,2,2-trifluoro-1-methyl-ethyl ester and the mixture was heated at 90° C. for 16 h. The mixture was then cooled to RT, poured onto water and extracted 3 times with ethyl acetate. The combined organic phases were dried with Na2SO4. Evaporation in vacuo followed by chromatography on silica gel (eluant: dichloromethane) afforded the title compound. MS (m/e): 359.2 (M+NH4+, 80%), 342.0 (M+H+, 100%)

WORKUP

后处理

  1. temperatureThe mixture was then cooled to RT
  2. additionpoured onto water
  3. extractionextracted 3 times with ethyl acetate
  4. dry with materialThe combined organic phases were dried with Na2SO4
  5. customEvaporation in vacuo