反应详情

温度

70 °C

To a solution of 5-(3-bromopropylidene)-10,11-dihydro-5H-dibenzo[a,d]cycloheptene (described in JP 48-030064) (200 mg) in DMF (10 ml) were added 4-(4-chlorophenyl)-4-hydroxypiperidine (230 mg), potassium carbonate (360 mg), and potassium iodide (50 mg). The mixture was stirred at 70° C. for 24 hours. Water and ethyl acetate were added to the reaction mixture, the organic layer was separated and washed with saturated aqueous sodium chloride, and dried with magnesium sulfate. The solvent was distilled off under reduced pressure. The residue was purified by silica gel chromatography eluting with ethyl acetate-hexane (1:1) to give the titled compound (250 mg). 1H-NMR (CDCl3) d: 1.65–2.11(5H,m), 2.32–3.10(8H,m), 3.22–3.67(4H,m), 5.87(1H,t), 7.03–7.44(12H,m). MS m/z: 444(M+1).

1. customthe organic layer was separated
2. washwashed with saturated aqueous sodium chloride
3. dry with materialdried with magnesium sulfate
4. distillationThe solvent was distilled off under reduced pressure
5. customThe residue was purified by silica gel chromatography
6. washeluting with ethyl acetate-hexane (1:1)