Reaktion #63586

Reaktionsgleichung

α-(3-chloropropyl)-4-fluoro-α-(4-fluorophenyl)benzeneacetonitrile

sulfuric acid

water

→

3,3-bis(4-fluorophenyl)tetrahydro-2H-pyran-2-one

Lösungsmittel

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturrefluxed for 24 hours
2. 2
   EinengenThe reaction mixture was concentrated to about 100 parts
3. 3
   Extraktionthe product was extracted with methylbenzene
4. 4
   WaschenThe extract was washed with water
5. 5
   Sonstigedried
6. 6
   Filtrationfiltered
7. 7
   Sonstigeevaporated
8. 8
   FiltrationThe product was filtered off
9. 9
   Sonstigecrystallized from 2,2'-oxybispropane

Vorschrift

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 15).

Quelle