反应详情

3-Chloropropyl 2-pyridyl ketone (1.8 g) and thiourea (0.8 g) are dissolved in ethanol (50 ml), and the solution is refluxed with stirring for 2 hours. To the mixture are added 1-methyl-5-chloro-1,2,3,4-tetrazole (1.2 g) and 10% aqueous sodium hydroxide (5 ml), and the mixture is refluxed for 3 hours. After evaporating ethanol under reduced pressure, water is added to the residue. The mixture is extracted with chloroform, and the extract is washed with water and saturated aqueous sodium chloride and dried over magnesium sulfate. After chloroform is distilled off, the residue is purified by column chromatography (Wakogel C-200, eluting agent, chloroform), followed by recrystallized from hexane-ether to give 1-methyl-5-[3-(2-pyridylcarbonyl)propyl]thio-1,2,3,4-tetrazole (0.2 g) as colorless crystals, m.p. 73°-75° C.

1. temperaturethe solution is refluxed
2. temperaturethe mixture is refluxed for 3 hours
3. customAfter evaporating ethanol under reduced pressure, water
4. additionis added to the residue
5. extractionThe mixture is extracted with chloroform
6. washthe extract is washed with water and saturated aqueous sodium chloride
7. dry with materialdried over magnesium sulfate
8. distillationAfter chloroform is distilled off
9. customthe residue is purified by column chromatography (Wakogel C-200, eluting agent, chloroform)
10. customby recrystallized from hexane-ether