反应详情

Under cooling with ice, 1-benzhydrylazetidin-3-ol (718 mg) in tetrahydrofuran (8 mL) was added dropwise to a suspension of 60% sodium hydride (144 mg) in N,N-dimethylformamide (8 mL), and the resultant mixture was stirred for 20 minutes. Methyl iodide (0.23 mL) was added to the reaction mixture, followed by stirring at room temperature overnight. The reaction mixture was partitioned between cold saturated aqueous ammonium chloride and ethyl acetate. The organic layer was washed with saturated brine, and then dried over magnesium sulfate anhydrate, followed by filtration. The solvent was evaporated under reduced pressure. The residue was purified through silica gel column chromatography (hexane-ethyl acetate), to thereby give the title compound as an oily product (680 mg, 90%).

1. customThe reaction mixture was partitioned between cold saturated aqueous ammonium chloride and ethyl acetate
2. washThe organic layer was washed with saturated brine
3. dry with materialdried over magnesium sulfate anhydrate
4. filtrationfollowed by filtration
5. customThe solvent was evaporated under reduced pressure
6. customThe residue was purified through silica gel column chromatography (hexane-ethyl acetate)