反应详情

A suspension of 10% Pd/C (200 mg), tert-butyl 4-(4-((4-((2-(1-(methoxycarbonyl)cyclopropyl)phenyl)ethynyl)-5-(trifluoromethyl)pyrimidin-2-yl)amino)phenyl)piperidine-1-carboxylate (A3) (0.302 g, 0.487 mmol) and Et3N (1.0 mL) in DMF (10 mL) was stirred under an atmosphere of hydrogen for 16 hours. The resulting mixture was diluted with EtOAc (60 mL) and filtered through Celite. The filtrate was evaporated under reduced pressure to give the title compound A4 as a yellow oil (494 mg, 99%); 1H NMR (400 MHz, d6-DMSO) δ 10.15 (s, 1H), 8.68 (s, 1H), 7.67 (d, J=8.6 Hz, 2H), 7.33-7.26 (m, 3H), 7.22-7.17 (m, 3H), 4.07 (d, J=11.6 Hz, 2H), 3.49 (s, 3H), 3.15-3.07 (m, 2H), 3.07-3.00 (m, 2H), 2.86-2.75 (m, peaks obscured by solvent), 2.70-2.58 (m, 1H), 1.74 (d, J=11.3 Hz, 2H), 1.58 (d, J=3.4 Hz, 2H), 1.48 (dt, J=12.6, 6.2 Hz, 2H), 1.42 (s, 9H), 1.21 (s, 2H). LCMS-A: rt 7.175 min; m/z 625 [M+H]+.

1. filtrationfiltered through Celite
2. customThe filtrate was evaporated under reduced pressure