HRID1607534

反应详情

EQUATION

反应方程式

HRID 1607534 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

In 165 ml of methanol, 4.1 g of 2-phenylthio-6-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one was dissolved. A dispersion of 40.3 g of OXONE® suspended in 165 ml of water was added to the methanol solution, and the resulting mixture was warmed to 60° C. and stirred for 2 hours. After cooling, chloroform was added for extraction, the organic layer was washed with a sodium thiosulfate aqueous solution, a sodium hydrogen carbonate aqueous solution and water respectively. After the organic layer was dried over anhydrous sodium sulfate, the solvent was distilled off. The residue was recrystallized from a toluene/ethanol (1:1) mixture and thus 1.2 g of 2-benzenesulfonyl-6-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one was obtained.

WORKUP

后处理

  1. temperatureAfter cooling
  2. washthe organic layer was washed with a sodium thiosulfate aqueous solution
  3. dry with materialAfter the organic layer was dried over anhydrous sodium sulfate
  4. distillationthe solvent was distilled off
  5. customThe residue was recrystallized from a toluene/ethanol (1:1) mixture