反应详情

In the above formulae, Bn is a benzyl group. First, copper(II) acetate monohydrate is dissolved in acetic acid, zinc powder is added to this solution, and allyl benzyl ether dissolved in dry diethyl ether was added thereto. Trichloroacetyl chloride and phosphoryl trichloride dissolved in dry diethyl ether are added dropwise to the solution. The reaction solution is refluxed, stirred, returned to room temperature, and filtered. The filtrate is washed, dehydrated, concentrated, and then to the residue are added acetic acid and zinc powder, followed by stirring under reflux. After the reaction solution is filtered, the filtrate is concentrated, the residue is dissolved in ethyl acetate, and zinc powder precipitated upon neutralization is filtered off. This filtrate is separated, washed with saturated NaHCO3 solution and brine, and the organic phase is dehydrated, concentrated, and evaporated under reduced pressure to remove the unreacted allyl benzyl ether, thereby to obtain 3-(benzyloxymethyl)cyclobutanone.

1. additionwas added
2. additionare added dropwise to the solution
3. temperatureThe reaction solution is refluxed
4. customreturned to room temperature
5. filtrationfiltered
6. washThe filtrate is washed
7. concentrationconcentrated
8. additionto the residue are added acetic acid and zinc powder
9. stirringby stirring
10. temperatureunder reflux
11. filtrationAfter the reaction solution is filtered
12. concentrationthe filtrate is concentrated
13. dissolutionthe residue is dissolved in ethyl acetate
14. customzinc powder precipitated upon neutralization
15. filtrationis filtered off
16. customThis filtrate is separated
17. washwashed with saturated NaHCO3 solution and brine
18. concentrationconcentrated
19. customevaporated under reduced pressure
20. customto remove the unreacted allyl benzyl ether