反应详情

A solution of 1-(1,1-dimethylethyl)-4-(5-fluoro-2-(methyloxy)-3-[{phenylmethyl)oxy]phenyl}-3-methyl-1H-pyrazol-5-amine (25 g, 0.0652 mol) in a mixture of THF-ethyl acetate (1:1, 300 mL) was hydrogenated over 10% Pd—C (2.5 g) at 40 Psi for 2 h. The catalyst was filtered off, and the filtrate was concentrated. The resulting crude was triturated with diethyl ether; a white solid was precipitated. It was collected by filtration, washed with an additional portion of diethyl ether and dried in vacuo to give 17.8 g of 3-[5-amino-1-(1,1-dimethylethyl)-3-methyl-1H-pyrazol-4-yl]-5-fluoro-2-(methyloxy)phenol (93%). 1H NMR (400 MHz, DMSO-d6): δ 9.63 (s, 1H), 6.56 (dd, 1H), 6.38 (dd, 1H), 4.44 (s, 2H), 3.37 (s, 3H), 1.98 (s, 3H), 1.56 (s, 9H); MS (EI) for C15H20FN3O2: 294 (MH+)

1. filtrationThe catalyst was filtered off
2. concentrationthe filtrate was concentrated
3. customThe resulting crude was triturated with diethyl ether
4. customa white solid was precipitated
5. filtrationIt was collected by filtration
6. washwashed with an additional portion of diethyl ether
7. customdried in vacuo