反应详情

A solution of compound 72 (350 mg, 1.46 mmol) in methanol (10 mL) was added to Raney Nickel (slurry in H2O, 50 mg) in a round bottom flask. The suspension was heated at reflux for 10 minutes then filtered through a pad of celite. The celite pad washed with methanol (20 mL). The filtrate was concentrated and the residue was subjected to silica gel chromatography (CH2Cl2 to MeOH:CH2Cl2, 5:95) to give compound 73 (300 mg, 98.4%) as a viscous oil. 1H NMR (DMSO-d6) δ 8.81 (d, J=2.6 Hz, 1H), 8.53-8.51 (m, 1H), 8.02-7.99 (m, 1H), 7.56-7.54 (m, 2H), 7.32 (d, J=8.7 Hz, 1H), 6.77 (d, J=1.9 Hz, 1H), 6.59 (dd, J=2.1, 6.7 Hz, 1H), 6.47 (d, J=3.4 Hz, 1H), 4.72 (brs, 2H); ESI-MS (m/z, %): 210 (M+1, 100%).

1. temperatureThe suspension was heated
2. temperatureat reflux for 10 minutes
3. filtrationthen filtered through a pad of celite
4. washThe celite pad washed with methanol (20 mL)
5. concentrationThe filtrate was concentrated