反应详情

To a round bottom flask was added 6-chloro-N2-methylpyridine-2,3-diamine (1-2) (2.043 g, 12.96 mmol), sulfamide (2.69 g, 28.0 mmol), and anhydrous pyridine (20 ml). The reaction mixture was refluxed at 125 C in a hot oil bath with stirring under an atmosphere of nitrogen with a water cooled reflux condenser attached overnight (16 hours). The reaction mixture was then cooled to room temperature and suspended in EtOAc (250 mL) & 6N HCl in water (250 mL) and filtered. Filtrate was then separated, organics dried over sodium sulfate, filtered & concentrated. The resulting residue was then purified with silica gel chromatography (0-20% Isopropanol/DCM) & concentrated to yield 5-chloro-3-methyl-1,3-dihydro[1,2,5]thiadiazolo[3,4-b]pyridine 2,2-dioxide (23-1). HRMS (M+H)+: observed=219.9946, calculated=219.9942.

1. temperatureThe reaction mixture was refluxed at 125 C in a hot oil bath
2. temperaturecooled
3. temperaturereflux condenser
4. custom(16 hours)
5. filtration6N HCl in water (250 mL) and filtered
6. customFiltrate was then separated
7. dry with materialorganics dried over sodium sulfate
8. filtrationfiltered
9. concentrationconcentrated
10. customThe resulting residue was then purified with silica gel chromatography (0-20% Isopropanol/DCM)
11. concentrationconcentrated