反应详情

To a solution of racemic tert-butyl 4-(6-benzyl-2-(2,6-dimethylphenyl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-yl)-(trans)-2,5-dimethylpiperazine-1-carboxylate (0.43 g, 0.794 mmol) in THF (9 mL) and water (3 mL) was added acetic acid (227 μL, 3.97 mmol) and 20% Pd(OH)2 on carbon (50% wet) (0.167 g, 0.238 mmol). The flask was evacuated and purged with hydrogen gas and then placed under a hydrogen atmosphere. After stirring at rt for 1 h the mixture was filtered over Celite®, and the Celite® pad was washed with EtOAc. The filtrate was washed with sat aq NaHCO3 and then the organic layer was dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure to obtain racemic tert-butyl 4-(2-(2,6-dimethylphenyl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-yl)-(trans)-2,5-dimethylpiperazine-1-carboxylate. MS (ESI+) m/z 452.3 (M+H)+.

1. customThe flask was evacuated
2. custompurged with hydrogen gas
3. filtrationwas filtered over Celite®
4. washthe Celite® pad was washed with EtOAc
5. washThe filtrate was washed with sat aq NaHCO3
6. dry with materialthe organic layer was dried over anhydrous sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure