反应详情

温度

70 °C

To a solution of 4-{[(3-cyclopentylpropanoyl)(2,2-dimethyl-4-oxo-4H-1,3-benzodioxin-6-yl)amino]methyl}-N-(4-phenoxybenzyl)benzamide (200 mg) in EtOH (3 mL) was added an aqueous solution (0.071 mL, 1N). The mixture was heated at 70° C. for 3 h. After cooling to rt, an aqueous solution of HCl (2 mL, 1N) was added and the resulting reaction mixture was extracted (EtOAc). The combined organic layers were washed with water, brine, dried over MgSO4, filtered and evaporated to give the title compound as a white powder (160 mg, 85%). 1H NMR (DMSO-d) δ 8.99 (t, J=6.0 Hz, 1H), 7.82 (d, J=8.2 Hz, 2H), 7.50 (d, J=2.6 Hz, 1H), 7.42-7.06 (m, 8H), 7.03-6.89 (m, 5H), 4.85 (s, 2H), 4.45 (s, 1H), 4.43 (s, 1H), 3.40 (brs, 1H), 2.05 (t, J=7.5 Hz, 2H), 1.70-1.32 (m, 9H), 1.00-0.81 (m, 2H). M+(ESI): 593.0; M−(ESI): 591.0. HPLC, Rt: 4.9 min purity: 99.3%).

1. temperatureAfter cooling to rt
2. customthe resulting reaction mixture
3. extractionwas extracted (EtOAc)
4. washThe combined organic layers were washed with water, brine
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. customevaporated