HRID1252093

反应详情

EQUATION

反应方程式

HRID 1252093 的结构方程式

PROCEDURE

实验过程

A mixture of 6.1 g of 2-hexylthio-7-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one, 9.1 g of a 30% hydrogen peroxide solution and 14 ml of acetic acid was heated to 65°-75° C. and stirred for 2 hours and 15 minutes. After cooling, water was added to the mixture and the resulting mixture was extracted with chloroform. The organic layer was washed with a sodium thiosulfate and water respectively, and dried over anhydrous sodium sulfate anhydrate. The solvent was distilled off. The residue was recrystallized from ethanol and thus 3.2 g of 2-hexanesulfonyl-7-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one was obtained. m.p. 111°-115° C. Yield 45%.

WORKUP

后处理

  1. temperaturewas heated to 65°-75° C.
  2. temperatureAfter cooling
  3. extractionthe resulting mixture was extracted with chloroform
  4. washThe organic layer was washed with a sodium thiosulfate and water respectively
  5. dry with materialdried over anhydrous sodium sulfate anhydrate
  6. distillationThe solvent was distilled off
  7. customThe residue was recrystallized from ethanol