反应详情

A mixture of methyl 1-[3-(benzyloxy)propyl]-4-[5-({2-[(4-{[ethoxy(hydroxy)phosphoryl]methyl}-2-methoxyphenyl)amino]-5-(trifluoromethyl)pyrimidin-4-yl}amino)-6-(methylcarbamoyl)pyridin-2-yl]-1H-pyrrole-2-carboxylate (Compound 38B, 582 mg, 0.717 mmol) and Palladium 10% wt. on Calcium Carbonate:Carbon black (63.4 mg, 0.031 mmol) in EtOH (11.4 mL), was evacuated and purged with d with H2(g) (3×) and left to stir overnight at rt for 16 hrs. The reaction mixture was filtered and concentrated in vacuo to a 330 mg of a solid which was used without further purification (64%). 1H NMR (400 MHz, CD3OD) δ 8.88-9.02 (m, 1H), 8.27 (s, 1H), 7.89 (s, 1H), 7.72 (d, J=6.3 Hz, 1H), 7.56-7.62 (m, 1H), 7.52 (d, J=1.5 Hz, 1H), 7.09 (s, 1H), 6.91 (d, J=8.1 Hz, 1H), 4.47 (t, J=6.8 Hz, 2H), 3.85-3.92 (m, 5H), 3.85 (br. s., 3H), 3.54-3.61 (m, 2H), 3.03 (d, J=22.0 Hz, 2H), 2.95-2.99 (m, 3H), 1.97-2.06 (m, 2H), 1.17 (t, J=7.1 Hz, 3H). MS (ESI): m/z=722.60 [M+H]+. UPLC: tR=1.22 min (UPLC-TOF: polar—2 min).

1. custompurged with d with H2(g) (3×)
2. waitleft
3. filtrationThe reaction mixture was filtered
4. concentrationconcentrated in vacuo to a 330 mg of a solid which
5. customwas used without further purification (64%)
6. customtR=1.22 min (UPLC-TOF: polar—2 min)