反应详情

The 1-[4-(methylsulfonyl)phenyl]-4,4′-bipiperidine (80 mg, 0.25 mmol, prepared as for Example 1, Step 2) and cesium carbonate (243 mg, 0.75 mmol) were slurried in NMP (0.5 ml) and the 2-chloro-3-methylpyrazine (38 mg, 0.30 mmol) added. The mixture was stirred at 150 C overnight. The slurry was diluted with 15% saturated sodium bicarbonate:water (40 ml) and extracted with DCM (3×25 ml). The combined organic fraction was washed with 4:1 water:saturated sodium bicarbonate (2×), brine, dried over magnesium sulfate, filtered, and the volatiles removed in vac. The crude material was purified by chromatography on silica gel with 5% acetone:DCM to yield the titled compound.

1. extractionwater (40 ml) and extracted with DCM (3×25 ml)
2. washThe combined organic fraction was washed with 4:1 water
3. dry with materialsaturated sodium bicarbonate (2×), brine, dried over magnesium sulfate
4. filtrationfiltered
5. customthe volatiles removed in vac
6. customThe crude material was purified by chromatography on silica gel with 5% acetone