反应详情

1.80 g of 2-(2-{2-[2-(3-methoxymethoxyphenyl)ethyl]phenoxy}ethyl]-1-methylpyrrolidine [prepared as described in step (a) above] were dissolved in 20 ml of a 4N solution of hydrogen chloride in dioxane, and the solution was allowed to stand at room temperature for 30 minutes. At the end of this time, the mixture was concentrated by distillation under reduced pressure, and the resulting oily residue was dissolved in 20 ml of methylene chloride. Ethyl acetate was slowly added to the solution until it just began to show signs of turbidity. The mixture was then allowed to stand overnight at room temperature. The crystals which precipitated were collected by filtration and dried in vacuo, to give 1.25 g (yield 71%) of the title compound as colorless crystals, melting at 68°-70° C.

1. concentrationAt the end of this time, the mixture was concentrated by distillation under reduced pressure
2. dissolutionthe resulting oily residue was dissolved in 20 ml of methylene chloride
3. additionEthyl acetate was slowly added to the solution until it
4. waitto stand overnight at room temperature
5. customThe crystals which precipitated
6. filtrationwere collected by filtration
7. customdried in vacuo