反应详情

温度

22 °C

To a stirred solution of Intermediate 4 (4.4 g) in 1:1 methanol/water (300 ml) was added potassium carbonate (17.5 g). The mixture was stirred at 22° C. for 36 h before the volatiles were evaporated in vacuo. The residue was dissolved in water and the solution extracted with dichloromethane (×3). The combined organic extracts were washed with saturated aqueous sodium chloride solution, dried over magnesium sulphate and filtered before evaporation of the solvent in vacuo. The residue was dissolved in methanol and purified by solid phase extraction (Isolute SCX sulphonic acid column), initially washing the cartridge with methanol before eluting with 10% 0.880 ammonia solution in methanol to give the title compound as a colourless oil (2.27 g).

1. customwere evaporated in vacuo
2. dissolutionThe residue was dissolved in water
3. extractionthe solution extracted with dichloromethane (×3)
4. washThe combined organic extracts were washed with saturated aqueous sodium chloride solution
5. dry with materialdried over magnesium sulphate
6. filtrationfiltered before evaporation of the solvent in vacuo
7. dissolutionThe residue was dissolved in methanol
8. custompurified by solid phase extraction (Isolute SCX sulphonic acid column)
9. washinitially washing the cartridge with methanol
10. washbefore eluting with 10% 0.880 ammonia solution in methanol