反应详情

To a stirred solution of 74.4 parts of 2-bromo-1-(2-naphthalenyl)-1-ethanone in 240 parts of butanol are added successively 3 parts of 4-methylbenzenesulfonic acid and 270 parts of benzene. Then there are added dropwise 28 parts of 1,2-butanediol. Upon completion, stirring is continued overnight at reflux temperature. The reaction mixture is evaporated. The residue is dissolved in 2,2'-oxybispropane and the solution is stirred with a diluted sodium hydroxide solution. The layers are separated and the aqueous phase is extracted with 2,2'-oxybispropane. The extract is neutralized with water, dried, filtered and evaporated. The oily residue is crystallized from methanol. The product is filtered off and recrystallized from methanol, yielding 41 parts of 2-(bromomethyl)-2-(2-naphthalenyl)-1,3-dioxolane; mp. 64° C.

1. temperatureat reflux temperature
2. customThe reaction mixture is evaporated
3. dissolutionThe residue is dissolved in 2,2'-oxybispropane
4. stirringthe solution is stirred with a diluted sodium hydroxide solution
5. customThe layers are separated
6. extractionthe aqueous phase is extracted with 2,2'-oxybispropane
7. customdried
8. filtrationfiltered
9. customevaporated
10. customThe oily residue is crystallized from methanol
11. filtrationThe product is filtered off
12. customrecrystallized from methanol