反应详情

温度

150 °C

A mixture of 2-Chloro-6-(4-{[4-(2-oxo-2,3-dihydro-1H-benzimidazol-1-yl)piperidin-1-yl]methyl}phenyl]-5-phenylnicotinonitrile (2-6, 0.040 g, 0.077 mmol) and methylamine (2M in THF, 0.192 mL, 0.385 mmol) in i-PrOH (1 mL) were heated@150° C. for 15 min. in the microwave. The mixture was concentrated, taken up in DMF and purified by reverse phase HPLC (6-1; 5% CH3CN: 95% H2O+0.01% TFA to 95% CH3CN: 5% H2O+0.01% TFA). 1H-NMR (500 MHz, d6 DMSO) δ 10.93 (s, 1H), 9.59 (bs, 1H), 8.00 (s, 1H), 7.37-7.47 (m, 4H), 7.18-7.37 (m, 5H), 7.12 (dd, J=1.96, 8.06, 2H), 6.95-7.05 (m, 3H), 4.43-4.53 (m, 1H), 4.32 (d, J=5.00, 2H), 3.47 (d, J=10.99, 2H), 3.10-3.25 (m, 2H), 2.94 (d, J=4.39, 3H), 255-2.69 (m, 2H), 1.92 (d, J=11.48, 2H). HRMS m/z (M+H) Calcd: 515.2554, found: 515.2552.

1. concentrationThe mixture was concentrated
2. custompurified by reverse phase HPLC (6-1; 5% CH3CN: 95% H2O+0.01% TFA to 95% CH3CN: 5% H2O+0.01% TFA)