HRID1252093
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperaturewas heated to 65°-75° C.
- temperatureAfter cooling
- extractionthe resulting mixture was extracted with chloroform
- washThe organic layer was washed with a sodium thiosulfate and water respectively
- dry with materialdried over anhydrous sodium sulfate anhydrate
- distillationThe solvent was distilled off
- customThe residue was recrystallized from ethanol