反应详情

温度

120 °C

1-(4-Bromophenyl)-9-methyl-2-(2,3,4-trifluorophenoxy)-1,9-dihydro-6H-purin-6-one (68 mg, 0.1507 mmol), Zn(CN)2 (10.6 mg, 0.0904 mmol), Pd2(dba)3 (4.1 mg, 0.0045 mmol) and 1,1′-bis(diphenylphosphino)ferrocene (5.0 mg, 0.0090 mmol) are added to DMF (1.2 mL) and H2O (0.012 mL). The mixture is purged with N2 for 3 min and then heated at 120° C. for 18 h. The mixture is passed through celite. Water (30 mL) is added and the resulting mixture is extracted with CH2Cl2 (50 mL×4). After drying the CH2Cl2 over MgSO4, the solvent is removed in vacuo. The crude product is purified by column chromatography (MeOH:CH2Cl2=2:98) to afford the title compound as a brown solid. 1H NMR (400 MHz, CDCl3) 7.86 (2H, d, J 8), 7.65 (1H, s), 7.53 (2h, d, J 8), 6.95 (2H, m), 3.59 (3H, s). MS (M+1): 398.03; RT=1.22 min.

1. customThe mixture is purged with N2 for 3 min
2. additionWater (30 mL) is added
3. extractionthe resulting mixture is extracted with CH2Cl2 (50 mL×4)
4. dry with materialAfter drying the CH2Cl2 over MgSO4
5. customthe solvent is removed in vacuo
6. customThe crude product is purified by column chromatography (MeOH:CH2Cl2=2:98)