反应详情

1-Methyl-5-chloro-1,2,3,4-tetrazole (1.4 g) and 3-mercaptopropyl cyclohexyl ketone (1.9 g) are dissolved in methanol (50 ml) and potassium hydroxide (0.8 g) is added to the solution. The mixture is refluxed for 5 hours. Methanol is distilled off and water is added to the residue. The mixture is extracted with chloroform. The chloroform solution is washed with dil. aqueous sodium hydroxide, water and saturated aqueous sodium chloride and dried over sodium sulfate. Chloroform is distilled off and the residue is purified by column chromatography (Wakogel C-200, eluant: chloroform) to obtain 1-methyl-5-(3-cyclohexylcarbonylpropyl)thio-1,2,3,4-tetrazole (0.6 g) as colorless liquid, nD12 =1.5267.

1. temperatureThe mixture is refluxed for 5 hours
2. distillationMethanol is distilled off
3. additionwater is added to the residue
4. extractionThe mixture is extracted with chloroform
5. washThe chloroform solution is washed with dil. aqueous sodium hydroxide, water and saturated aqueous sodium chloride
6. dry with materialdried over sodium sulfate
7. distillationChloroform is distilled off
8. customthe residue is purified by column chromatography (Wakogel C-200, eluant: chloroform)