反应详情

To a solution of 2-{[2-(benzyloxy)-4,6-dimethylpyridin-3-yl]methyl}-8-chloro-7-(difluoromethoxy)-3,4-dihydroisoquinolin-1(2H)-one (1i, 0.08 g, 0.169 mmol) in CH2Cl2 (10 mL) was added TFA (10 mL) at room temperature. The resulting mixture was stirred at room temperature for 4 hours. The mixture was concentrated under vacuum to give a residue, which was dissolved in CH2Cl2 (20 mL) and then washed with sat. NaHCO3 (5 mL), brine (5 mL), dried over Na2SO4, and concentrated under vacuum. The residue was purified by prep. TLC (EtOAc) to obtain the title compound (Example 1, 43.1 mg, 67%) as a white solid. 1H NMR (400 MHz, methanol-d4) δ 7.36-7.34 (m, 1H), 7.24-7.22 (m, 1H), 7.00-6.63 (m, 1H), 6.11 (s, 1H), 4.76 (s, 2H), 3.51-3.48 (m, 2H), 2.90-2.87 (m, 2H), 2.29 (s, 3H), 2.25 (s, 3H); MS 382.9 [M+1].

1. concentrationThe mixture was concentrated under vacuum
2. customto give a residue, which
3. washwashed with sat. NaHCO3 (5 mL), brine (5 mL)
4. dry with materialdried over Na2SO4
5. concentrationconcentrated under vacuum
6. customThe residue was purified by prep