反应详情

温度

0 °C

To a solution of 2-mercapto-6-methylbenzonitrile (1.00 g, 6.71 mmol) in ethyl acetate (10 mL), bromine (1.05 g, 6.60 mmol) was added dropwise at 0° C. The reaction mixture was allowed to stir at 0° C. for 3 h. The reaction mixture was then allowed to warm to room temperature, followed by heating at reflux for 3 h. The reaction mixture was concentrated under reduced pressure. Crystallization of the crude mixture with hexanes gave 3-bromo-4-methylbenzo[d]isothiazole (2.7 g), which was carried forward without further purification. MW=228 confirmed by LC-MS, tr=6.82 min (Method E) MH+=229.

1. temperatureto warm to room temperature
2. temperatureby heating
3. temperatureat reflux for 3 h
4. concentrationThe reaction mixture was concentrated under reduced pressure
5. customCrystallization of the crude mixture with hexanes