反应详情

温度

80 °C

3-Hydroxyisoquinoline (170 mg, 1.17 mmol), 1-benzo[b]thiophen-4-yl-4-(3-chloropropyl)piperazine (290 mg, 1.0 mmol), and potassium carbonate (200 mg, 1.45 mmol) were added to dimethylformamide (8 ml), followed by stirring at 80° C. for 7 hours. The reaction mixture was cooled to room temperature, then water was added thereto and the reaction mixture was extracted with ethyl acetate. The organic phase was washed with water, dried over magnesium sulfate, and concentrated under reduced pressure after filtration. The residue was purified by basic silica gel column chromatography (n-hexane:ethyl acetate=9:1), and concentrated under reduced pressure. The resulting residue was dissolved in ethanol (2 ml), and 1N—HCl—ethanol solution (0.5 ml) was added thereto. Insoluble matters produced were filtered out and dried to obtain 3-[3-(4-benzo[b]thiophen-4-yl-piperazin-1-yl)propoxy]isoquinoline hydrochloride (160 mg, yield: 37%) as white powder.

1. temperatureThe reaction mixture was cooled to room temperature
2. extractionthe reaction mixture was extracted with ethyl acetate
3. washThe organic phase was washed with water
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. filtrationafter filtration
7. customThe residue was purified by basic silica gel column chromatography (n-hexane:ethyl acetate=9:1)
8. concentrationconcentrated under reduced pressure
9. dissolutionThe resulting residue was dissolved in ethanol (2 ml)
10. addition1N—HCl—ethanol solution (0.5 ml) was added
11. customInsoluble matters produced
12. filtrationwere filtered out
13. customdried