HRID2425055

反应详情

EQUATION

反应方程式

HRID 2425055 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 0.442 g 5-sulfamoyl-thiophene-2-carboxylic acid methyl ester in 8 ml tetrahydrofuran was added 0.044 g lithiumborohydride and the mixture was stirred at room temperature for 20 h. To the resulting mixture was added an other 0.088 g lithiumborohydride and the mixture was stirred at room temperature for 2 h and at reflux for 20 h. The resulting suspension was partitioned between water and ethyl acetate. The phases were separated and the organic phase was purified by chromatography on silica gel with ethyl acetate to yield 0.300 g of the title compound as white crystals melting at 70-71° C.

WORKUP

后处理

  1. stirringthe mixture was stirred at room temperature for 2 h
  2. temperatureat reflux for 20 h
  3. customThe resulting suspension was partitioned between water and ethyl acetate
  4. customThe phases were separated
  5. customthe organic phase was purified by chromatography on silica gel with ethyl acetate