反应详情

To a mixed solution of a commercially available product of 1-(diphenylmethyl)azetidin-3-one (1.00 g, 4.21 mmol), THF (20 mL) and acetic acid (1.00 mL) was added methylpiperazine (561 μL, 5.05 mmol) at room temperature. The resultant mixture was stirred at room temperature for 15 minutes. To the reaction mixture was added sodium triacetoxyborohydride (1.79 g, 8.42 mmol) at room temperature, and the resultant mixture was stirred at room temperature for 2 hours and 15 minutes. Sodium hydrogen carbonate and water were added to the reaction mixture, and the resultant mixture was extracted with ethyl acetate. An organic layer was washed with saturated brine, then dried over anhydrous magnesium sulfate, and then filtrated. The solvent was evaporated under a reduced pressure, and the resultant residue was purified by silica gel column chromatography (ethyl acetate-methanol) and then further purified by NH silica gel column chromatography (heptane:ethyl acetate=1:1) to give the title compound (1.21 g, yield: 89%).

1. extractionthe resultant mixture was extracted with ethyl acetate
2. washAn organic layer was washed with saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. filtrationfiltrated
5. customThe solvent was evaporated under a reduced pressure
6. customthe resultant residue was purified by silica gel column chromatography (ethyl acetate-methanol)
7. customfurther purified by NH silica gel column chromatography (heptane:ethyl acetate=1:1)