反应详情

A mixture of tert-butyl 3-hydroxy-4,4-dimethoxypiperidine-1-carboxylate [synthesized by the method described in Tetrahedron Lett., 46(3), 447-450 (2005)] (10 g, 38.3 mmol), pyridine (100 mL) and acetic anhydride (18.1 mL, 192 mmol) was stirred at 70° C. overnight. The reaction solution was cooled to room temperature, diluted with ethyl acetate, washed with 1 N hydrochloric acid and brine, and dried over magnesium sulfate. Thereafter, the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (Elution solvent: hexane/ethyl acetate=4/1) to obtain 9.65 g of the title compound as a colorless oil (83%).

1. customsynthesized by the method
2. washwashed with 1 N hydrochloric acid and brine
3. dry with materialdried over magnesium sulfate
4. customThereafter, the solvent was evaporated under reduced pressure
5. customThe resulting residue was purified by silica gel column chromatography (Elution solvent: hexane/ethyl acetate=4/1)