反应详情

温度

130 °C

A mixture of 2-acetylamino-5-chlorothiazole (1.76 g), 5-mercapto1-methyl-1H-tetrazole (1.2 g) and potassium carbonate (2 g) in N,N-dimethylformamide (40 ml) was heated at 130° C. for 3 hours with stirring. The reaction mixture was concentrated under reduced pressure and the residue was triturated with water. The precipitates were collected by filtration, washed with water and dried vacuo to give solid. The solid was subjected to column chromatography on silica gel (silica gel 60, 70-230 mesh; Merck: 150 g) and eluted with a mixture of chloroform and methanol (10:1). The fractions containing the objective compound were combined and concentrated under reduced pressure to give 2-acetylamino-5-(1-methyl-1H-tetrazol-5-ylthio)thiazole (2.1 g, yield: 82.0%).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. customthe residue was triturated with water
3. filtrationThe precipitates were collected by filtration
4. washwashed with water
5. customdried vacuo
6. customto give solid
7. washeluted with a mixture of chloroform and methanol (10:1)
8. additionThe fractions containing the objective compound
9. concentrationconcentrated under reduced pressure