反应详情

To a solution of Compound 40 (0.21 g, 0.36 mmol, Example 5) in DMF (3 mL) was added methyl 3-aminopropanoate (0.12 g, 0.89 mmol), HATU (0.20 g, 0.53 mmol) and DIEA (0.37 mL, 2.1 mmol). The resulting mixture was stirred at rt for 16 h and poured into water (20 mL). The aqueous layer was extracted with DCM (2×20 mL). The combined organic layers were dried over MgSO4 and filtered. Upon removal of the solvent, the resultant residue was purified by flash chromatography on silica gel (40-100% EtOAc/heptane) to give compound 7a as a red solid. 1H-NMR (400 MHz, CDCl3) δ (ppm): 8.12 (d, J=8.8 Hz, 1H), 8.07 (d, J=8.6 Hz, 1H), 7.92-8.03 (m, 4H), 7.84 (d, J=8.6 Hz, 2H), 7.78 (d, J=8.1 Hz, 1H), 7.65-7.76 (m, 3H), 7.46-7.54 (m, 1H), 6.97 (t, J=6.0 Hz, 1H), 6.13 (d, J=5.6 Hz, 1H), 4.06-4.13 (m, 4H), 3.96-4.03 (m, 4H), 3.76-3.83 (m, 2H), 3.75 (s, 3H), 2.71 (t, J=5.9 Hz, 2H).

1. extractionThe aqueous layer was extracted with DCM (2×20 mL)
2. dry with materialThe combined organic layers were dried over MgSO4
3. filtrationfiltered
4. customUpon removal of the solvent
5. customthe resultant residue was purified by flash chromatography on silica gel (40-100% EtOAc/heptane)