Reaktion #63574

Reaktionsgleichung

water

2-chloroethanol

sulfuric acid

4-fluoro-α-(4-fluorophenyl)benzenemethanol

→

1,1'-[(2-chloroethoxy)methylene]bis[4-fluorobenzene]

Lösungsmittel

benzene

benzene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated on a water-bath
2. 2
   workup.ADDITIONAfter the addition
3. 3
   Temperaturrefluxed for 4 hours
4. 4
   TemperaturAfter cooling the reaction mixture
5. 5
   SonstigeThe benzene layer was separated
6. 6
   Trocknendried over calcium chloride
7. 7
   Sonstigeevaporated
8. 8
   workup.DISTILLATIONThe residue was distilled in vacuo

Vorschrift

A mixture of 20 parts of 2-chloroethanol, 3 parts of sulfuric acid and 16 parts of benzene was heated on a water-bath. Then there were added dropwise 35 parts of 4-fluoro-α-(4-fluorophenyl)benzenemethanol dissolved in 32 parts of benzene. After the addition was complete, the whole was stirred and refluxed for 4 hours. After cooling the reaction mixture was poured into water. The benzene layer was separated, dried over calcium chloride and evaporated. The residue was distilled in vacuo, yielding 35 parts of 1,1'-[(2-chloroethoxy)methylene]bis[4-fluorobenzene]; bp. 164°-166° C. at 1.5 mm. pressure; nD20 : 1.5462; d2020 : 1.2290 (intermediate 1).

Quelle