HRID1606076
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 4.8 g. 3-propylsulphinyl-1,2,4-triazole, 4.48 g. diethylcarbamoyl chloride, 40 ml. dry tetrahydrofuran and 6 ml. dry triethylamine was refluxed under anhydrous conditions for 5 hours. The cooled reaction mixture was filtered to remove triethylamine hydrochloride. The filtrate was diluted with petroleum ether (b.p. 40° - 60°C.), causing the deposition of an oil which gradually solidified. The solid product was collected and recrystallized from a mixture of ether and petroleum ether (b.p. 40° - 60°C.) to give 1-diethylcarbamoyl-3-propylsulphinyl-1,2,4-triazole, m.p. 50.5° - 51.5°C.
WORKUP
后处理
- additionA mixture of 4.8 g
- customThe cooled reaction mixture
- filtrationwas filtered
- customto remove triethylamine hydrochloride
- additionThe filtrate was diluted with petroleum ether (b.p. 40° - 60°C.)
- customThe solid product was collected
- customrecrystallized from a mixture of ether and petroleum ether (b.p. 40° - 60°C.)