HRID1758296

反应详情

EQUATION

反应方程式

HRID 1758296 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 (1.2 g) is dissolved in acetone (50 ml). To the solution are added 3-bromopropyl phenyl sulfide (2.5 g) and potassium carbonate (1.5 g) and the mixture is refluxed for 4 hours. Acetone is distilled off and water is added to the residue. The mixture is extracted with chloroform. The chloroform solution is washed with saturated aqueous sodium chloride and dried over magnesium sulfate. Chloroform is distilled off and the residue is purified by column chromatography (Kieselgel 60). The column is eluted with benzenechloroform (3:2) to obtain 1-methyl-5-(3-phenylthiopropyl)thio-1,2,3,4-tetrazole (1.8 g) as colorless liquid, nD18 =1.6008.

WORKUP

后处理

  1. temperaturethe mixture is refluxed for 4 hours
  2. distillationAcetone is distilled off
  3. additionwater is added to the residue
  4. extractionThe mixture is extracted with chloroform
  5. washThe chloroform solution is washed with saturated aqueous sodium chloride
  6. dry with materialdried over magnesium sulfate
  7. distillationChloroform is distilled off
  8. customthe residue is purified by column chromatography (Kieselgel 60)
  9. washThe column is eluted with benzenechloroform (3:2)