反应详情

2-(4-Bromophenethyl)-benzyl bromide, 27.0 g. (0.0764 mole) and 6.2 g. (0.0954 mole) of potassium cyanide are suspended in 180 ml. of 95% ethanol and the mixture is stirred at reflux for 2 hours. Ethanol, 70 ml. of 95%, is added and stirring at reflux is continued for 2 hours. The precipitate is removed by filtration and the ethanolic filtrate evaporated under reduced pressure. The residual brown oil is dissolved in benzene and the solution is washed thoroughly with water and dried over anhydrous sodium sulfate. Evaporation of the benzene under reduced pressure leaves the product as the residual dark yellow oil that slowly solidifies to an oily solid. Recrystallization from cyclohexane-petroleum ether gives purified material, m.p. 59°-60.5° C. Vapor phase chromatography indicates a purity of approximately 99%.

1. temperatureat reflux for 2 hours
2. additionof 95%, is added
3. temperatureat reflux
4. customThe precipitate is removed by filtration
5. customthe ethanolic filtrate evaporated under reduced pressure
6. dissolutionThe residual brown oil is dissolved in benzene
7. washthe solution is washed thoroughly with water
8. dry with materialdried over anhydrous sodium sulfate
9. customEvaporation of the benzene under reduced pressure
10. customleaves the product as the residual dark yellow oil that
11. customRecrystallization from cyclohexane-petroleum ether
12. customgives
13. custompurified material, m.p. 59°-60.5° C