反应详情

To a solution of the product of step 1 (470 mg) in acetic acid (5 ml) was added 48% aqueous HBr (3 ml) at 10° C. The reaction mixture was warmed to room temperature, and stirred for 12 hours. Water and ethyl acetate were added to the reaction mixture and neutralized with dilute NaOH solution. The organic layer was separated and washed with saturated aqueous sodium chloride, and dried over magnesium sulfate. The solvent was distilled off under reduced pressure. The residue was purified by silica gel chromatography eluting with ethyl acetate-hexane (1:4) to give 4-bromo-1-(3-methoxyphenyl)-1-(3-pyridinyl)-1-butene (560 mg).

1. customThe organic layer was separated
2. washwashed with saturated aqueous sodium chloride
3. dry with materialdried over 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 (1:4)