HRID501241

反应详情

EQUATION

反应方程式

HRID 501241 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

The mixture of 300 mg of 2-chloro-5-trifluoromethyl-[1,3,4]thiadiazol, 300 mg of N-(5-sulfamoyl-indan-2-yl)-acetamide, 1.8 g cesium carbonate und 10 ml of NMP was stirred at 70° C. for 3 hours. After cooling to room temperature 50 ml of water were added and with 2N hydrochloric acid a pH=3 was adjusted. The product was extracted twice with 30 ml of ethyl acetate, the organic layer was washed with 20 ml of water, dried over sodium sulfate and evaporated in vacuo. The resulting crude material was purified by column chromatography (silica gel, eluent: dichloromethane:methanol=90:10).

WORKUP

后处理

  1. extractionThe product was extracted twice with 30 ml of ethyl acetate
  2. washthe organic layer was washed with 20 ml of water
  3. dry with materialdried over sodium sulfate
  4. customevaporated in vacuo
  5. customThe resulting crude material was purified by column chromatography (silica gel, eluent: dichloromethane:methanol=90:10)