反应详情

The tert-butyl 1′-(6-chloropyrimidin-4-yl)-4,4′-bipiperidine-1-carboxylate (50 mg, 0.13 mmol, prepared as described for Example 13) and sodium acetate (11 mg, 0.13 mmol) were dissolved in methanol (1.3 ml), 10% palladium on carbon (14 mg) added and the solution stirred overnight under a hydrogen atmosphere. The solution was diluted with 4:1 water:saturated sodium bicarbonate (40 ml) and extracted with ethyl acetate (3×25 ml). The combined organic fraction was washed with brine, dried over magnesium sulfate, filtered, and the volatiles removed in vac. The crude material was purified by chromatography on silica gel with 35% acetone:hexanes to yield the titled compound.

1. extractionsaturated sodium bicarbonate (40 ml) and extracted with ethyl acetate (3×25 ml)
2. washThe combined organic fraction was washed with brine
3. dry with materialdried over magnesium sulfate
4. filtrationfiltered
5. customthe volatiles removed in vac
6. customThe crude material was purified by chromatography on silica gel with 35% acetone