HRID1758317

反应详情

EQUATION

反应方程式

HRID 1758317 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturethe mixture is refluxed for 4 hours
  2. distillationAfter acetone is distilled off
  3. additionwater is added to the residue
  4. extractionextracted with chloroform
  5. washThe chloroform solution is washed with saturated aqueous sodium chloride
  6. dry with materialdried over sodium sulfate
  7. distillationAfter chloform is distilled off
  8. customthe residue is purified by column chromatography (neutral alumina, made by Merck)
  9. washeluted with n-hexane