反应详情

1-Methyl-5-[4,4-ethylenedioxy-4-(2-pyridyl)butyl]thio-1,2,3,4-tetrazole (0.7 g) is dissolved in acetic acid (5 ml). Water (2.5 ml) and conc. hydrochloric acid (0.5 ml) are added to the solution and the mixture is heated on a water bath for 1 hour. Water is added to the reaction mixture and the mixture is extracted with chloroform. The chloroform solution is washed with water, saturated aqueous sodium bicarbonate and saturated aqueous sodium chloride and dried over magnesium sulfate. Chloroform is distilled off and the residue is purified by silica gel column chromatography (Kieselgel 60). The column is eluted with benzene-ether (10:1) and the product is recrystallized from hexane-ether to obtain 1-methyl-5-[3-(2-pyridylcarbonyl)propyl]thio-1,2,3,4-tetrazole, (0.5 g) as colorless needles, m.p. 73°-75° C.

1. temperaturethe mixture is heated on a water bath for 1 hour
2. extractionthe mixture is extracted with chloroform
3. washThe chloroform solution is washed with water, saturated aqueous sodium bicarbonate and saturated aqueous sodium chloride
4. dry with materialdried over magnesium sulfate
5. distillationChloroform is distilled off
6. customthe residue is purified by silica gel column chromatography (Kieselgel 60)
7. washThe column is eluted with benzene-ether (10:1)
8. customthe product is recrystallized from hexane-ether