反应详情

60% Sodium hydride (27 mg, 0.68 mmol) was washed with hexane under argon atmosphere, and then suspended in dimethyl sulfoxide (5 ml). The obtained suspension was stirred at room temperature for 30 minutes. 5,11-Dihydrodibenzo[b,e][1,4]oxazepine (122 mg, 0.68 mmol) was added to the suspension, and they were stirred at room temperature for 20 minutes and then at 50° C. for 30 minutes. A solution of (R)-3-chloro-1-(3-methoxyphenethyl)homopiperidine (182 mg, 0.68 mmol) in dimethyl sulfoxide (3 ml) was added dropwise into the obtained solution, and they were stirred at 50° C. for 150 minutes. The reaction liquid was distributed in saturated aqueous sodium hydrogencarbonate solution and ethyl acetate. The organic layer was dried, and the solvent was evaporated under reduce pressure. The obtained residue was subjected to silica gel column chromatography. The product was eluted with hexane and ethyl acetate (10:1) and then with hexane and ethyl acetate (4:1). The appropriate fractions were combined, and the solvent was evaporated under reduced pressure to obtain (R)-5,11-dihydro-5-[1-(3-methoxyphenethyl)piperidine-2-ylmethyl] dibenzo[b,e][1,4]oxazepine in the form of a light yellow oil (78 mg, 30%).

1. stirringwere stirred at room temperature for 20 minutes
2. waitat 50° C. for 30 minutes
3. stirringwere stirred at 50° C. for 150 minutes
4. customThe reaction liquid
5. customThe organic layer was dried
6. customthe solvent was evaporated
7. washThe product was eluted with hexane and ethyl acetate (10:1)
8. customthe solvent was evaporated under reduced pressure