反应详情

温度

50 °C

A mixture of chloromethyl-(4-nitrophenyl)diketone (2 g), thiourea (1.5 g) and sodium acetate (1.6 g) in ethanol (20 ml) was heated at 50° C. for 4 hours with stirring. The mixture was concentrated in vacuo and the residue was triturated with water. The precipitates were collected by filtration, washed with water and dried in vacuo to give solid. The solid was subjected to column chromatography on silica gel (silica gel 60, 70-230 mesh; Merck: 100 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-amino-4-(4-nitrobenzoyl)thiazole (0.71 g, yield: 32.4%). mp: 194°-198° C. (dec.) IR (Nujol): 3300-3450, 1660, 1600, 1520, 1350 cm-1

1. concentrationThe mixture was concentrated in vacuo
2. customthe residue was triturated with water
3. filtrationThe precipitates were collected by filtration
4. washwashed with water
5. customdried in 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