反应详情

127 mg of dibenzoyl peroxide were added to a solution of 8.79 g of 2-methyl-5-fluorobenzothiazole and 20.6 g of N-bromosuccinimide in 88 ml of carbon tetrachloride at room temperature and the resulting mixture was stirred under reflux for 6 hours. At the end of this time, the reaction mixture was filtered and the resulting filtrate was concentrated by evaporation under reduced pressure to give a crude crystalline solid which was purified by column chromatography through silica gel using a 10:1 by volume mixture of hexane and ethyl acetate to give 850 mg (yield 7%) of the title compound as a solid.

1. temperatureunder reflux for 6 hours
2. filtrationAt the end of this time, the reaction mixture was filtered
3. concentrationthe resulting filtrate was concentrated by evaporation under reduced pressure
4. customto give a crude crystalline solid which
5. customwas purified by column chromatography through silica gel using a 10:1
6. additionby volume mixture of hexane and ethyl acetate