反应详情

In an autoclave, 8-benzyl-3-pyrimidin-2-yl-8-azabicyclo[3.2.1]octan-3-ol (5.0 g, 17 mmol), palladium on charcoal (3,5 g, 5% Pd/C, 50% water wet) ethanol (27.5 ml) and 2N HCl (2.5 ml) were mixed and hydrogenated under a pressure of 0.5 to 1.5 bar at 50° C. The reaction was followed by HPLC. After complete reaction (6 to 8 h) the mixture was filtered and the residue washed with ethanol. The filtrate was concentrated to dryness under vacuum at 50° and the crude product is purified by column chromatography (90 g silica gel, methanol:ammonia (25%) 50:1). Yield: 1.8 g (52%) as free base. Assay (HPLC): 99% area.

1. customAfter complete reaction (6 to 8 h) the mixture
2. filtrationwas filtered
3. washthe residue washed with ethanol
4. concentrationThe filtrate was concentrated to dryness under vacuum at 50°
5. customthe crude product is purified by column chromatography (90 g silica gel, methanol:ammonia (25%) 50:1)