HRID354041

反应详情

EQUATION

反应方程式

HRID 354041 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-methylthio-1,3,4-thiadiazole-5-thiol (1 mmole) in THF (5 mL) was treated with sodium hydride (60%, 1.1 mmole) at 0° C. and the resulting mixture was stirred at room temperature for 30 min. The reaction was then cooled to 0° C. and treated with diethylphosphonomethyl trifluoromethanesulfonate (1.1 mmole). After stirring at room temperature for 12 h, the reaction was quenched with saturated ammonium chloride. Extraction and chromatography gave 2-methylthio-5-diethylphosphonomethylthio-1,3,4-thiadiazole as an oil.

WORKUP

后处理

  1. temperatureThe reaction was then cooled to 0° C.
  2. stirringAfter stirring at room temperature for 12 h
  3. customthe reaction was quenched with saturated ammonium chloride
  4. extractionExtraction and chromatography