反应详情

温度

120 °C

7-(2-Fluoro-phenoxy)-4-hydroxy-1-iodo-isoquinoline-3-carboxylic acid methyl ester (100 mg, 0.23 mmol) and CuCN (41 mg, 0.46 mmol) were suspended in DMF (1.0 mL). The resulting mixture was heated at 120° C. for 7 minutes and then cooled to room temperature. The reaction crude was poured into CH2Cl2 (30 mL) and stirred vigorously for 10 minutes at room temperature. The resulting suspension was filtered through a pad of celite and the filtrate was washed with H2O and brine sequentially. The organic layer was dried over MgSO4, concentrated, and purified by flash chromatography (0-50% EtOAc/hexanes) to give the title compound in 75 mg. 1H NMR (CDCl3, 200 MHz): δ=12.27 (s, 1H), 8.45 (d, 1H, J=9.0 Hz), 7.63-7.57 (m, 1H), 7.50-7.48 (m, 1H), 7.29-7.20 (m, 4H), 4.11 (s, 3H).

1. temperaturecooled to room temperature
2. customThe reaction crude
3. filtrationThe resulting suspension was filtered through a pad of celite
4. washthe filtrate was washed with H2O and brine sequentially
5. dry with materialThe organic layer was dried over MgSO4
6. concentrationconcentrated
7. custompurified by flash chromatography (0-50% EtOAc/hexanes)