反应详情

A solution of 3-[4-(azetidine-1-carbonyl)-2-chloro-phenoxy]-5-[(3S)-1-methyl-2-oxo-pyrrolidin-3-yl]oxy-N-(5-methylpyrazin-2-yl)benzamide (Intermediate 22) (120 mg, 0.22 mmol) and 10% palladium on carbon (20 mg, catalytic) in THF (5 mL) and ethanol (5 mL) was stirred under an atmosphere of hydrogen for 16 hours. The palladium on carbon was removed by filtration and the filtrate evaporated under reduced pressure. The residue was dissolved in ethyl acetate (30 mL), washed with water (10 mL), brine (10 mL), dried (MgSO4), filtered and evaporated under reduced pressure to give product (98 mg, 89%). 1H NMR δ (300 MHz, CDCl3) 2.12-2.26 (m, 1H), 2.36 (quintet, 2H), 2.52-2.67 (m, 4H), 2.94 (s, 3H), 3.35-3.57 (m, 2H), 4.19-4.42 (m, 4H), 4.93 (t, 1H), 6.93 (s, 1H), 7.03 (d, 2H), 7.20 (s, 1H), 7.42 (s, 1H), 7.66 (d, 2H), 8.15 (s, 1H), 8.54 (s, 1H), 9.52 (s, 1H); m/z 502 (M+H)+.

1. customThe palladium on carbon was removed by filtration
2. customthe filtrate evaporated under reduced pressure
3. dissolutionThe residue was dissolved in ethyl acetate (30 mL)
4. washwashed with water (10 mL), brine (10 mL)
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. customevaporated under reduced pressure