反应详情

To a mixture of 5-chloro-6-[(1R)-2,2,2-trifluoro-1-methylethoxy]pyridin-3-ol (Preparation 235, 360 mg, 0.86 mmol) and 4-methylphenyl 5-chloro-2,4-difluorobenzoate (Preparation 12, 242 mg, 0.86 mmol) in DMSO (2 mL) was added K2CO3 (237 mg, 1.7 mmol) at room temperature under N2 and the resulting mixture was stirred for 5 hours. The reaction was quenched with water and extracted with DCM (3×5 mL). The mixture was filtered through a phase separation cartridge. The combined organic phases were washed with brine (3 mL) and filtered through another phase separation cartridge. The filtrate was dried by N2 blowing to give a crude product. The crude product was purified by silica gel column chromatography eluting with 0-40% EtOAc in heptane to give the title compound (429 mg, 99%) as colourless gum.

1. customThe reaction was quenched with water
2. extractionextracted with DCM (3×5 mL)
3. filtrationThe mixture was filtered through a phase separation cartridge
4. washThe combined organic phases were washed with brine (3 mL)
5. filtrationfiltered through another phase separation cartridge
6. dry with materialThe filtrate was dried by N2 blowing
7. customto give a crude product
8. customThe crude product was purified by silica gel column chromatography
9. washeluting with 0-40% EtOAc in heptane