反应详情

1-Methyl-5-mercapto-1,2,3,4-tetrazole (0.01 mol), potassium carbonate (0.015 mol) and α-chloroacetone (0.015 mol) 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. The filtrate is concentrated under reduced pressure and the residue is purified by silica gel column chromatography [Kieselgel 60, eluant: benzene-ether (10:1)] and the product is recrystallized from methanol-ether to obtain 1-methyl-5-acetylmethylthio-1,2,3,4-tetrazole (yield 48%) as colorless needles, m.p. 31° 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 filtrate is concentrated 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 methanol-ether