反应详情

A mixture of 3-hydroxy-5-[(3S)-1-methyl-2-oxo-pyrrolidin-3-yl]oxy-N-(5-methylpyrazin-2-yl)benzamide (Intermediate 18) (136 mg, 0.4 mmol), azetidin-1-yl-(3-chloro-4-fluoro-phenyl)methanone (CAS no. 863454-79-9) (128 mg, 0.6 mmol) and potassium carbonate (111 mg, 0.8 mmol) in DMA (5 mL) was stirred at 120° C. for 16 hours. The solution was evaporated under reduced pressure, then the residue was dissolved in ethyl acetate (40 mL), washed with water (2×20 mL) and brine (10 mL), then dried (MgSO4), filtered and the solvent removed under reduced pressure. The residue was purified by chromatography on silica eluting with 0-4% methanol/DCM to afford the product (120 mg, 56%). m/z 536 (M+H)+.

1. customThe solution was evaporated under reduced pressure
2. dissolutionthe residue was dissolved in ethyl acetate (40 mL)
3. washwashed with water (2×20 mL) and brine (10 mL)
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customthe solvent removed under reduced pressure
7. customThe residue was purified by chromatography on silica eluting with 0-4% methanol/DCM