HRID917323

反应详情

EQUATION

反应方程式

HRID 917323 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into 2 ml of N,N-dimethylformamide was dissolved 215 mg of 2-chlorobenzyl alcohol, 59 mg of sodium hydride (60% in oil) was added thereto under ice-cooling. After stirring for 30 minutes, a solution of 250 mg of 5-chloro-3-methylthio-1,2,4-thiadiazole in 2 ml of N,N-dimethylformamide was added dropwise into the mixture and the reaction mixture was stirred for 0.5 hour under ice-cooling and for 2 hours at room temperature. The reaction mixture was added to saturated sodium chloride aqueous solution, and extracted with t-butyl methyl ether. The organic layer was concentrated, and the residue obtained was subjected to silica gel column chromatography to give 188 mg of 5-(2-chlorobenzyloxy)-3-methylthio-1,2,4-thiadiazole (hereinafter, referred to as the present compound (2)).

WORKUP

后处理

  1. additionwas added
  2. temperatureunder ice-cooling
  3. stirringthe reaction mixture was stirred for 0.5 hour under ice-
  4. extractionextracted with t-butyl methyl ether
  5. concentrationThe organic layer was concentrated
  6. customthe residue obtained