反应详情

温度

95 °C

To a mixture of 2-methyl-thiazole-4-carbonitrile (3.0 g, 24.1 mmol), N-bromosuccinimide (4.3 g, 24.1 mmol) in CCl4 (50 mL) was added benzoyl peroxide (0.583 g, 0.10 mmol). The resulting mixture was stirred at 95° C. for 15 h, concentrated under reduced pressure, diluted with EtOAc (100 mL) and washed with saturated Na2S2O3 (50 mL), NaHCO3 (50 mL) and brine (20 mL). The organic phase was dried over sodium sulfate and concentrated under reduced pressure. The crude residue was purified via silica gel column chromatography using EtOAc/n-hexane as eluent to afford the title compound (4.6 g, 83%) as yellow oil. Rf0.39 (silica gel,EtOAc/hexane,3/7).

1. concentrationconcentrated under reduced pressure
2. additiondiluted with EtOAc (100 mL)
3. washwashed with saturated Na2S2O3 (50 mL), NaHCO3 (50 mL) and brine (20 mL)
4. dry with materialThe organic phase was dried over sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe crude residue was purified via silica gel column chromatography