反应详情

To a stirred solution of 74.4 parts of 2-bromo-1-(2-naphthalenyl)-1-ethanone in 240 parts of a 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-ethanediol. 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 extra ct 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