反应详情

To a solution (or suspension) of 2-(5-chloropyrazin-2-ylcarbonylamino)-5-fluoro-N-(5-chloropyridin-2-yl)benzamide (Intermediate A-1, 10 g, 24.62 mmol) in DMSO (30 mL) was added 1-Boc-hexahydro-1,4-diazepine (9.86 g, 49.23 mmol) and pyridine (2.4 mL, 30 mmol). The reaction mixture was stirred for one hour at room temperature before it was heated in a sealed tube at 75–80° C. for 18 h. The mixture was cooled to room temperature, diluted with ethyl acetate (800 mL), washed with saturated aqueous citric acid solution (3×200 mL), water (200 mL), saturated sodium bicarbonate solution (2×200 mL), and dried over magnesium sulfate. Activated charcoal (3 g) was added to decolorize the product. Evaporation of the solvent under vacuum provided 13.9 g of crude product. Ether (150 mL) was added to this solid, the mixture was sonicated 20 min, and the solids were filtered and dried under vacuum to afford the title compound as a solid which was analytically pure. Yield=12.6 g

1. temperaturewas heated in a sealed tube at 75–80° C. for 18 h
2. temperatureThe mixture was cooled to room temperature
3. washwashed with saturated aqueous citric acid solution (3×200 mL), water (200 mL), saturated sodium bicarbonate solution (2×200 mL)
4. dry with materialdried over magnesium sulfate
5. additionActivated charcoal (3 g) was added
6. customEvaporation of the solvent under vacuum
7. customprovided 13.9 g of crude product
8. customthe mixture was sonicated 20 min
9. filtrationthe solids were filtered
10. customdried under vacuum