反应详情

温度

22 °C

To a stirred solution of Intermediate 19 (3.3 g) in N,N-dimethylformamide (50 ml) under nitrogen was added potassium carbonate (2.46 g) and sodium iodide (2.12 g). A solution of 3,4-dichlorobenzyl chloride (2 ml) in N,N-dimethylformamide (10 ml) was added dropwise to the mixture. The mixture was stirred at 22° C. for 18 h before the volatiles were removed in vacuo. The residue was partitioned between dichloromethane (100 ml) and saturated aqueous sodium carbonate solution (50 ml). The organic phase was subsequently washed with additional saturated aqueous sodium carbonate solution (2×50 ml) and water (50 ml) before drying over magnesium sulphate, filtering and evaporation of the solventin vacuo to give a pale yellow oil. The oil was purified by Biotage flash chromatography on a 90 g silica cartridge eluting with 25% ethyl acetate in cyclohexane, to give the title compound as a colourless oil (2.97 g).

1. customwere removed in vacuo
2. customThe residue was partitioned between dichloromethane (100 ml) and saturated aqueous sodium carbonate solution (50 ml)
3. washThe organic phase was subsequently washed with additional saturated aqueous sodium carbonate solution (2×50 ml) and water (50 ml)
4. dry with materialbefore drying over magnesium sulphate
5. filtrationfiltering
6. customevaporation of the solventin vacuo
7. customto give a pale yellow oil
8. customThe oil was purified by Biotage flash chromatography on a 90 g silica cartridge
9. washeluting with 25% ethyl acetate in cyclohexane