反应详情

To a solution of ethyl 2-(((11-fluoro-2-(2-(4-fluorophenyl)-3-(methylcarbamoyl)-6-(N-methylmethylsulfonamido)benzofuran-5-yl)-6H-pyrido[2′,3′:5,6][1,3]oxazino[3,4-a]indol-6-yl)methyl)amino)acetate (35 mg, 0.048 mmol) in 1,4-dioxane/H2O (3.0 mL/0.5 mL) was added LiOH.H2O (20 mg, 0.45 mmol). The mixture was stirred at room temperature overnight. Then it was concentrated in vacuo, neutralized with HCl (aq. 5%), extracted with EtOAc. The organic layer was washed with brine, dried over Na2SO4 and concentrated to provide Compound 116 (30 mg, yield: 91%). 1H-NMR (DMSO-d6, 400 MHz) δ 8.58 (d, J=4.8 Hz, 1H), 8.00˜8.07 (m, 2H), 7.85 (s, 1H), 7.69 (d, J=8.8 Hz, 1H), 7.61 (d, J=8.4 Hz, 1H), 7.52 (d, J=8.4 Hz, 1H), 7.43 (t, J=8.8 Hz, 2H), 7.20˜7.29 (m, 1H), 7.09 (s, 1H), 6.89˜6.97 (m, 1H), 6.85 (br. s, 1H), 3.19 (s, 3H), 3.07 (m, 2H), 2.88 (s, 3H), 2.83 (s, 3H). MS (M+H)+: 702.

1. concentrationThen it was concentrated in vacuo
2. extractionextracted with EtOAc
3. washThe organic layer was washed with brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated