反应详情

A mixture of 4-bromo-2,5-dimethyl-1,3-benzothiazole (5.8 g, 24 mmol), N-bromosuccinimide (5.12 g, 28.7 mmol), and benzoyl peroxide (0.580 g, 2.40 mmol) in carbon tetrachloride (100 mL) was heated at reflux overnight. The mixture was diluted with dichloromethane, washed with 1 N NaOH, brine and dried over sodium sulfate, then concentrated under reduced pressure. The residue was purified on silica gel, eluting with 0% to 50% EtOAc in hexane, to give the desired product (5.70 g, 74%). LCMS calculated for C9H8Br2NS(M+H)÷: m/z=319.9; found: 319.8.

1. temperaturewas heated
2. temperatureat reflux overnight
3. washwashed with 1 N NaOH, brine
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified on silica gel
7. washeluting with 0% to 50% EtOAc in hexane