反应详情

A mixture of 5.8 parts of 3,3-bis(4-fluorophenyl)-tetrahydro-2H-pyran-2-one and 30 parts of a solution of hydrobromic acid in glacial acetic acid was stirred over week-end at room temperature. The reaction mixture was poured onto water. The precipitated product was filtered off and dissolved in 2,2'-oxybispropane. The organic phase was washed with water, dried, filtered and evaporated. The residue was boiled in a mixture of 42 parts of 2,2'-oxybispropane and 42 parts of petroleumether. The product was filtered off and crystallized from 2,2'-oxybispropane, yielding 1.27 parts of α-(3-bromopropyl)-4-fluoro-α-(4-fluorophenyl)benzeneacetic acid; mp. 161° C. (intermediate 22).

1. additionThe reaction mixture was poured onto water
2. filtrationThe precipitated product was filtered off
3. dissolutiondissolved in 2,2'-oxybispropane
4. washThe organic phase was washed with water
5. customdried
6. filtrationfiltered
7. customevaporated
8. additionThe residue was boiled in a mixture of 42 parts of 2,2'-oxybispropane and 42 parts of petroleumether
9. filtrationThe product was filtered off
10. customcrystallized from 2,2'-oxybispropane