反应详情

温度

125 °C

To a round bottom flask was added 4-bromo-N2-methylbenzene-1,2-diamine (1-2) (9.07 g, 45.1 mmol), sulfamide (8.84 g, 92 mmol), and finally anhydrous pyridine (75 mL). The reaction mixture was then heated to 125° C. while stirring in a hot oil bath with a water cooled reflux condenser attached under an atmosphere of nitrogen for 14 hours. The crude reaction mixture was then allowed to cool to room temperature, suspended in ethyl acetate and added 6N HCl until pH <3. Crude mixture was then filtered. Filtrate organics were separated, then washed with 6N HCl twice dried over sodium sulfate, filtered, and concentrated to give 6-bromo-1-methyl-1,3-dihydro-2,1,3-benzothiadiazole 2,2-dioxide (1-3). HRMS (M+H)+: observed=262.9486, calculated=262.9484.

1. temperaturecooled
2. temperaturereflux condenser
3. customThe crude reaction mixture
4. temperatureto cool to room temperature
5. filtrationCrude mixture was then filtered
6. customFiltrate organics were separated
7. washwashed with 6N HCl
8. dry with materialtwice dried over sodium sulfate
9. filtrationfiltered
10. concentrationconcentrated