反应详情

1-Methyl-5-mercapto-1,2,3,4-tetrazole (1.2 g), potassium carbonate (2.1 g) and 3-chloropropyl 2-pyridyl ketone (2.8 g) are added to acetone (50 ml) and the mixture is refluxed with stirring for 2 hours. The reaction mixture is concentrated to dryness under reduced pressure and the residue is dissolved in chloroform. Insolubles are filtered off and the filtrated is concentrate under reduced pressure. The residue is purified by silica gel column chromatography (Kieselgel 60, eluant: 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 (yield 50%) as colorless needles, m.p. 73°-75° C.

1. temperaturethe mixture is refluxed
2. concentrationThe reaction mixture is concentrated to dryness under reduced pressure
3. dissolutionthe residue is dissolved in chloroform
4. filtrationInsolubles are filtered off
5. concentrationthe filtrated is concentrate under reduced pressure
6. customThe residue is purified by silica gel column chromatography (Kieselgel 60, eluant: benzene-ether (10:1))
7. customthe product is recrystallized from hexane-ether