反应详情

温度

80 °C

A steel clabe was charged with a mixture of compound 5 (400 mg, 1.39 mmol), KCN (362 mg, 5.57 mmol) in EtOH (4 mL) and H2O (4 mL). The mixture was heated at 80° C. for 24 h. The reaction mixture was cooled to room temperature and poured into ice (10 g) and filtered. The filter cake was washed with water (10 mL×2) and CH2Cl2 (10 mL×2), dried under reduced pressure to give compound 6 (440 mg, 78%) as a white solid. LC-MS tR=1.219 min in 2 min chromatography, MS (ESI) m/z 333, 335 [M+H]+; 1H NMR (DMSO 400 MHz): δ 10.82 (m, 1H), 8.52 (d, J=27.2 Hz, 1H), 7.53 (m, 1H), 7.34 (m, 2H), 5.78 (d, J=6.4 Hz, 2H), 2.61 (m, 4H), 2.23 (m, 2H).

1. temperatureThe reaction mixture was cooled to room temperature
2. filtrationfiltered
3. washThe filter cake was washed with water (10 mL×2) and CH2Cl2 (10 mL×2)
4. customdried under reduced pressure