反应详情

1-Methyl-5-chloro-1,2,3,4-tetrazole (2.4 g) is dissolved in ethanol (30 ml). Thiourea (1.5 g) is added to the solution and the mixture is refluxed for 2 hours. 3-Bromopropyl cyclohexyl ketone (4.7 g) and 10% aqueous sodium hydroxide (10 ml) are added to the mixture is further refluxed for 3 hours. Ethanol is distilled off and water is added to the residue. The mixture is extracted with chloroform. The chloroform solution is washed with water and then saturated aqueous sodium chloride and dried over magnesium 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 (1.4 g) as colorlss liquid, nD12 =1.5267.

1. temperaturethe mixture is refluxed for 2 hours
2. temperatureis further refluxed for 3 hours
3. distillationEthanol is distilled off
4. additionwater is added to the residue
5. extractionThe mixture is extracted with chloroform
6. washThe chloroform solution is washed with water
7. dry with materialsaturated aqueous sodium chloride and dried over magnesium sulfate
8. distillationChloroform is distilled off
9. customthe residue is purified by column chromatography (Wakogel C-200, eluant: chloroform)