反应详情

To a solution of [(2R)-2-(cyclopentylmethyl)-3-(2-{6-[(2R)-2,4-dimethyl-1-piperazinyl]-5-fluoro-2-methyl-4-pyrimidinyl}hydrazino)-3-oxopropyl][(phenylmethyl)oxy]formamide (15.60 g, 28.8 mmol) in methanol (115 mL) was added Pd/C (50% water, 3.1 g). The mixture was hydrogenated under balloon pressure for 2 h, and then filtered through a glass fiber filter. The solution was then concentrated in vacuo and azeotroped with EtOAc (100 mL). The resulting solid was triturated with 70% EtOAc in hexanes, and collected by vacuum filtration. The supernatant was concentrated in vacuo and crystallized from EtOAc-hexanes, and the solid was combined with the first crop of material. The combined solid was dried overnight under high vacuum to give [(2R)-2-(cyclopentylmethyl)-3-(2-{6-[(2R)-2,4-dimethyl-1-piperazinyl]-5-fluoro-2-methyl-4-pyrimidinyl}hydrazino)-3-oxopropyl]hydroxyformamide (8.15 g, 18.05 mmol, 62.7% yield) as a white solid. LCMS: (M+H)+: 451.8.

1. filtrationfiltered through a glass fiber
2. filtrationfilter
3. concentrationThe solution was then concentrated in vacuo
4. customazeotroped with EtOAc (100 mL)
5. customThe resulting solid was triturated with 70% EtOAc in hexanes
6. filtrationcollected by vacuum filtration
7. concentrationThe supernatant was concentrated in vacuo
8. customcrystallized from EtOAc-hexanes
9. customThe combined solid was dried overnight under high vacuum