反应详情

To a cooled (0° C.) solution of chlorosulfonic acid (58 mL) under vigorous stirring was added 5-bromo-2-pyridinamine (15 g, 86.7 mmol) portionwise. The reaction mixture was then heated at reflux for 3 hrs. Upon cooling to room temperature, the reaction mixture was poured over ice (˜100 g) with vigorous stirring. The resulting yellow precipitate was collected by suction filtration, washing with cold water and petroleum ether to provide the title compound as an orange-yellow solid (18.1 g, 77% yield). MS (ES)+ m/e 272.8 [M+H]+.

1. temperatureThe reaction mixture was then heated
2. temperatureat reflux for 3 hrs
3. filtrationThe resulting yellow precipitate was collected by suction filtration
4. washwashing with cold water and petroleum ether