反応 #63586

反応方程式

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

sulfuric acid

water

→

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

溶媒

acetic acid

反応条件

後処理

1. 1
   温度refluxed for 24 hours
2. 2
   濃縮The reaction mixture was concentrated to about 100 parts
3. 3
   抽出the product was extracted with methylbenzene
4. 4
   洗浄The extract was washed with water
5. 5
   その他dried
6. 6
   ろ過filtered
7. 7
   その他evaporated
8. 8
   ろ過The product was filtered off
9. 9
   その他crystallized from 2,2'-oxybispropane

実験手順

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).

出典