反应详情

A mixture of 4-(4-chlorophenyl)-5-methyl-2-phenylthiazole (35.1 g), N-bromosuccinimide (24.0 g), azobisisobutyronitrile (4.11 g) and carbon tetrachloride (400 mL) was stirred with heating under reflux for 3 hrs. The precipitated solid was removed by filtration and the organic layer was concentrated. The residue was purified by silica gel column chromatography. 5-(Bromomethyl)-4-(4-chlorophenyl)-2-phenylthiazole (30.8 g, 69%) was obtained as crystals from a fraction eluted with hexane-ethyl acetate (19:1, volume ratio). Recrystallization from ethyl acetate gave colorless prism crystals. melting point: 108–109° C.

1. temperaturewith heating
2. temperatureunder reflux for 3 hrs
3. customThe precipitated solid was removed by filtration
4. concentrationthe organic layer was concentrated
5. customThe residue was purified by silica gel column chromatography