反应详情

温度

120 °C

A mixture of 3-{[2-fluoro-1-(fluoromethyl)ethyl]oxy}-5-hydroxy-N-(1-methyl-1H-pyrazol-3-yl)benzamide (200 mg, 0.64 mmol), 5-(azetidin-1-ylcarbonyl)-2,3-dichloropyridine (164 mg, 0.71 mmol) and potassium carbonate (178 mg, 1.28 mmol) in acetonitrile (5 mL) was stirred in a ‘Biotage initiator Microwave’ at 120° C. for 4 hours. The solvent was removed in vacuo and the residue partitioned between ethyl acetate and water (100 mL), the organic layer washed with brine (50 mL), dried (MgSO4), filtered and the solvent removed in vacuo to give a brown oil which was chromatographed on silica, eluting with a gradient of 50-100% ethyl acetate in isohexane, to give the desired compound (237 mg).

1. customThe solvent was removed in vacuo
2. customthe residue partitioned between ethyl acetate and water (100 mL)
3. washthe organic layer washed with brine (50 mL)
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customthe solvent removed in vacuo
7. customto give a brown oil which
8. customwas chromatographed on silica
9. washeluting with a gradient of 50-100% ethyl acetate in isohexane