反应详情

To a solution of {2-(4-Chloro-phenyl)-2-[6-(3-methyl-1-trityl-1H-pyrazol-4-yl)-pyridin-3-yl]-vinyl}-methyl-(1-phenyl-ethyl)-amine in ethanol was added palladium, 10 wt. % on activated carbon and the reaction mixture was subjected to a hydrogen atmosphere for 17 hours. The mixture was filtered through Celite®, the mother liquor was concentrated, the residue was purified by column chromatography (SiO2), eluting with dichloromethane:methanol:acetic acid:water (240:20:3:2) to dichloromethane:methanol:acetic acid:water (90:18:3:2) to afford the title compound. LC/MS: (PS-A2) Rt 1.59 [M+H]+ 293.18. 1H NMR (Me-d3-OD) δ 2.35 (3H, s), 2.40 (3H, s), 3.25 (2H, s), 4.15-4.20 (1H, t), 7.10-7.18 (1H, m), 7.25 (4H, m), 7.45 (1H, d), 7.67 (1H, dd), 7.80 (1H, s), 8.38 (1H, s).

1. filtrationThe mixture was filtered through Celite®
2. concentrationthe mother liquor was concentrated
3. customthe residue was purified by column chromatography (SiO2)
4. washeluting with dichloromethane:methanol:acetic acid:water (240:20:3:2) to dichloromethane:methanol:acetic acid:water (90:18:3:2)