反应详情

A Grignard reagent prepared from magnesium (2.8 g, 116 mmol), 4-chloro-1-methylpiperidine (15.5 mL, 116 mmol), and THF (180 mL) was ice-cooled, and a THF (120 mL) solution of the compound obtained in Example 22 (18.5 g, 58 mmol) was added dropwise thereto. After allowing the mixture to react for 30 minutes, a saturated ammonium chloride was added thereto, and a product was extracted with ethyl acetate. The organic layer was sequentially washed with a saturated ammonium chloride and with a saturated sodium chloride solution, and then dried over anhydrous sodium sulfate, and the solvents were distilled off under a reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:2), to give 4.4 g (18%) of the captioned compound.

1. temperaturecooled
2. customto react for 30 minutes
3. extractiona product was extracted with ethyl acetate
4. washThe organic layer was sequentially washed with a saturated ammonium chloride and with a saturated sodium chloride solution
5. dry with materialdried over anhydrous sodium sulfate
6. distillationthe solvents were distilled off under a reduced pressure
7. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:2)