반응 #63586

반응 방정식

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

sulfuric acid

water

→

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

용매

acetic acid

반응 조건

후처리

1. 1
   온도refluxed for 24 hours
2. 2
   농축The reaction mixture was concentrated to about 100 parts
3. 3
   추출the product was extracted with methylbenzene
4. 4
   세척The extract was washed with water
5. 5
   기타dried
6. 6
   여과filtered
7. 7
   기타evaporated
8. 8
   여과The product was filtered off
9. 9
   기타crystallized from 2,2'-oxybispropane

실험 절차

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).

출처