反应详情

[(S)-3-(4-Fluoro-benzyl)-piperidin-1-yl]-[(3S,4R)-3-((R)-1-phenyl-ethylamino)-tetrahydro-pyran-4-yl]-methanone (1.10 g, 2.6 mmol), palladium hydroxide (20 weight % on carbon, dry basis; 440 mg) and ethanol (40 mL) were combined in a pressure bottle and shaken under a hydrogen atmosphere (55-60 psig) for 20 h . The mixture was filtered through Celite, and the solids were washed thoroughly with ethanol. The filtrate was concentrated to give the product as a glassy foam (803 mg, 96%), used without further purification. 1H NMR (300 mHz, CD3OD) δ7.22 (m, 2H), 7.04 (m, 2H), 4.50 and 4.30 (2m, 1H), 4.1-3.6 (3H), 3.5-3.4 (2H), 3.3-2.9 (2H), 2.8-2.4 (4H), 2.0-1.2 (7H), ESI MS: (M+H)+=321.2.

1. filtrationThe mixture was filtered through Celite
2. washthe solids were washed thoroughly with ethanol
3. concentrationThe filtrate was concentrated