反应详情

DIPEA (0.36 mL, 1.95 mmol) was added to a suspension of 3-fluoro-4-(3-[(1S)-2-hydroxy-1-methylethoxy]-5-{[(1-methyl-1H-pyrazol-3-yl)amino]carbonyl}phenoxy)benzoic acid (209 mg, 0.49 mmol), HATU (390 mg, 1.02 mmol) and piperidine (0.19 mL, 1.95 mmol) in DMF (3 mL), and the mixture stirred at ambient temperature for 24 hours. Water (30 mL) was added and the mixture extracted with diethyl ether/ethyl acetate 4:1 (3×20 mL). The combined organic extracts were washed with brine (30 mL), dried (MgSO4), and evaporated to a residue which was chromatographed on silica, eluting with a gradient of 0-20% methanol in ethyl acetate, to give the desired compound (116 mg).

1. extractionthe mixture extracted with diethyl ether/ethyl acetate 4:1 (3×20 mL)
2. washThe combined organic extracts were washed with brine (30 mL)
3. dry with materialdried (MgSO4)
4. customevaporated to a residue which
5. customwas chromatographed on silica
6. washeluting with a gradient of 0-20% methanol in ethyl acetate