HRID1758317
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-mercapto-1,2,3,4-tetrazole (2.4 g) and 2-chloromethylpyridine (2.6 g) are dissolved in acetone (50 ml). To the mixture are added potassium carbonate (2.8 g) and patassium iodide (0.1 g), and the mixture is refluxed for 4 hours. After acetone is distilled off, water is added to the residue and extracted with chloroform. The chloroform solution is washed with saturated aqueous sodium chloride and dried over sodium sulfate. After chloform is distilled off, the residue is purified by column chromatography (neutral alumina, made by Merck) and eluted with n-hexane to give 1-methyl-5-(2-pyridyl)methylthio-1,2,3,4-tetrazole (1.0 g) as colorless prisms (ethanol), m.p. 78°-81° C.
WORKUP
后处理
- temperaturethe mixture is refluxed for 4 hours
- distillationAfter acetone is distilled off
- additionwater is added to the residue
- extractionextracted with chloroform
- washThe chloroform solution is washed with saturated aqueous sodium chloride
- dry with materialdried over sodium sulfate
- distillationAfter chloform is distilled off
- customthe residue is purified by column chromatography (neutral alumina, made by Merck)
- washeluted with n-hexane