HRID1758341
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
1-Methyl-5-(3-chloropropylthio)-1,2,3,4-tetrazole (3.8 g) is dissolved in dimethylformamide (50 ml). To the mixture are added sodium iodide (3 g) and diethylamine (4.4 g) and the mixture is stirred at 60°-70° C. for 3 hours. Dimethylformamide is distilled off under reduced pressure, and the residue is purified by alumina column chromatography (basic alumina, made by Merk & Co.), followed by eluting with n-hexane to give 1-methyl-5-[3-(N,N-diethylamino)propylthio]-1,2,3,4-tetrazole (1.1 g), colorless liquid, nD25 =1.5040.
WORKUP
后处理
- distillationDimethylformamide is distilled off under reduced pressure
- customthe residue is purified by alumina column chromatography (basic alumina, made by Merk & Co.)
- washby eluting with n-hexane