反应详情

温度

25 °C

A suspension of tert-butyl 3-[4-(4-cyanophenyl)-4-(3,4-dimethoxyphenoxy)butyl]-3-azabicyclo[3.2.1]oct-8-yl(methyl)carbamate (see step (iv) above; 2.67 g, 4.86 mmol) in ethyl acetate saturated with HCl (60 mL) was stirred overnight at 25° C. under nitrogen. The mixture was partitioned with water (100 mL) and ethyl acetate (50 mL). The aqueous layer was washed with ethyl acetate (50 mL) before being separated, basified with saturated sodium bicarbonate (50 mL) and then extracted with dichloromethane (3×50 mL). The organic extracts were dried (Na2SO4), filtered, concentrated in vacuo and then chromatographed on silica gel, eluting with dichloromethane:methanol:concentrated ammonium hydroxide (92:7:1), to afford 1.32 g (61%) of the title compound as a yellow oil.

1. customThe mixture was partitioned with water (100 mL) and ethyl acetate (50 mL)
2. washThe aqueous layer was washed with ethyl acetate (50 mL)
3. custombefore being separated
4. extractionextracted with dichloromethane (3×50 mL)
5. dry with materialThe organic extracts were dried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customchromatographed on silica gel
9. washeluting with dichloromethane