反应详情

Prepared according to the procedure used to prepare methyl 2-(5-chloro-1H-indazol-7-yl)-2-((4-(4-fluorophenyl)-1-methylpiperidin-4-yl)methoxy)acetate trifluoroacetic acid salt using tert-butyl 4-(((5-chloro-1H-indazol-7-yl)(cyano)methoxy)methyl)-4-(4-fluorophenyl)piperidine-1-carboxylate as the starting material. After preparative HPLC, the product was still impure. The product was re-purified by column chromatography (2M ammonia in methanol/dichloromethane) to give the title compound as the freebase. 1H-NMR (CDCl3, 500 MHz) δ 9.51 (bs, 1H), 7.97 (s, 1H), 7.73 (d, J=1.8 Hz, 1H), 7.34 (dd, J=8.9, 5.2 Hz, 2H), 7.31 (s, 1H), 7.14 (m, 2H), 5.43 (s, 1H), 3.84 (d, J=8.6 Hz, 1H), 3.68 (d, J=8.5 Hz, 1H), 2.56 (m, 2H), 2.22 (m, 8H), 1.99 (m, 3H), 1.67 (bs, 6H). Mass spec.: 413.22 (MH)+.

1. customPrepared
2. customThe product was re-purified by column chromatography (2M ammonia in methanol/dichloromethane)