反应详情

温度

0 °C

To a solution of 3-(2,6-dichloro-3-nitro-phenyl)-1H-quinolin-2-one (0.21 g, 0.6266 mmol) in DMF (5.0 mL) is added HNa (30.1 mg, 60%, 0.752 mmol) and IMe (120.1 mg, 0.846 mmol) at 0° C. After the mixture is stirred for two hours at 0° C., the mixture is diluted with EtOAc and washed with saturated K2CO3, brine and water. The organic layer is dried, filtered and concentrated to give crude product, which is purified by flash silica gel column, eluting with CH2Cl2 (100%) gradient to CH2Cl2/MeOH (2N NH3) (95/5), t give the titled intermediate as a solid (78 mg, 35.8%).

1. washwashed with saturated K2CO3, brine and water
2. customThe organic layer is dried
3. filtrationfiltered
4. concentrationconcentrated
5. customto give crude product, which
6. customis purified by flash silica gel column
7. washeluting with CH2Cl2 (100%) gradient to CH2Cl2/MeOH (2N NH3) (95/5), t