反应详情

The tert-butyl-1′-(5-chloropyrazin-2-yl)-4,4′-bipiperidine-1-carboxylate (1.1 g, 2.9 mmol) was dissolved in 1:1 THF and NMP (30 mL) at r.t. Iron (III) acetylacetonate (512 mg, 1.45 mmol) was added under N2. Methyl magnesium bromide (3M, 3.9 mL, 11.6 mmol) was added dropwise and the mixture stirred for 15 min. An ice cooled solution of saturated ammonia chloride (30 mL, aq.) and ethyl acetate (30 mL) were added, the mixture shaken, and the phases separated. The organic phase was washed with brine (10 mL, ×1), dried over magnesium sulfate, filtered, and concentrated in vac. The residue was purified by chromatography on silica gel with 12.5% acetone: hexanes to yield the title compound.

1. stirringthe mixture shaken
2. customthe phases separated
3. washThe organic phase was washed with brine (10 mL, ×1)
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated in vac
7. customThe residue was purified by chromatography on silica gel with 12.5% acetone