反应详情

The compound (1.035 g) obtained in Example 518 was dissolved in methylene chloride (20 ml) and to the solution, triphenylphosphine (1.38 g) and carbon tetrabromide (1.74 g) were successively added under ice cooling. The reaction mixture was stirred for 30 min under ice cooling, then stirred at room temperature for 30 min and the solvent was distilled off under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent, n-hexane:ethyl acetate=5:1) to give 476.6 mg of the titled compound (yield, 36%).

1. additionwere successively added under ice cooling
2. stirringstirred at room temperature for 30 min
3. distillationthe solvent was distilled off under reduced pressure
4. customThe resulting residue was purified by silica gel column chromatography (eluent, n-hexane:ethyl acetate=5:1)