反应详情

A mixture of 3 parts of α-(3-chloropropyl)-4-fluoro-α-(4-fluorophenyl)benzeneacetonitrile, 92 parts of concentrated sulfuric acid, 50 parts of water and 50 parts of acetic acid was stirred and refluxed for 24 hours. The reaction mixture was concentrated to about 100 parts and the product was extracted with methylbenzene. The extract was washed with water, dried, filtered and evaporated. The residue was suspended in petroleumether. The product was filtered off and crystallized from 2,2'-oxybispropane, yielding 1.41 parts of 3,3-bis(4-fluorophenyl)tetrahydro-2H-pyran-2-one; mp. 122.4° C. (intermediate 21).

1. temperaturerefluxed for 24 hours
2. concentrationThe reaction mixture was concentrated to about 100 parts
3. extractionthe product was extracted with methylbenzene
4. washThe extract was washed with water
5. customdried
6. filtrationfiltered
7. customevaporated
8. filtrationThe product was filtered off
9. customcrystallized from 2,2'-oxybispropane