反应详情

A mixture of the above prepared 6-methyl-6′-(3-nitro-phenyl)-4-(4-trifluoromethyl-phenyl)-[2,2′]bipyridinyl (3.4 g, 7.81 mmol) in THF-EtOH 1:1 (100 mL) and 10% palladium on carbon (1 mol %) was hydrogenated (1 bar hydrogen) at 23° C. for 2 h. The catalyst was filtered off, washed with EtOH and the filtrate was completely evaporated totally to leave a crude product, which was purified by silica gel column chromatography with heptane/EtOAc, followed by trituration with diethyl ether to give the title compound as a white solid (2.55 g, 80%). MS (ISP) 406.3 [(M+H)+]; mp 167° C.

1. additionA mixture of the
2. customat 23° C.
3. customfor 2 h
4. filtrationThe catalyst was filtered off
5. washwashed with EtOH
6. customthe filtrate was completely evaporated totally
7. customto leave a crude product, which
8. customwas purified by silica gel column chromatography with heptane/EtOAc