Reaktion #655803

Reaktionsgleichung

HCl

2,3-dichloroanisole

2,6-difluoro benzoylchloride

AlCl3

→

2,3-dichloro-4-methoxy-2',6'-difluorobenzophenone

Lösungsmittel

1,2-dichloroethane

1,2-dichloroethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe organic layer is separated
2. 2
   Extraktionthe aqueous layer extracted with CHCl3
3. 3
   ExtraktionThe organic extract
4. 4
   Waschenis washed with water
5. 5
   Trocknendried (Na2SO4)
6. 6
   Sonstigeevaporated
7. 7
   Sonstigeto give an oil which
8. 8
   Sonstigecrystallizes from hexane

Vorschrift

To a solution of 24.6 g of 2,6-difluoro benzoylchloride in 100 ml of 1,2-dichloroethane, 18.5 g of AlCl3 is added in portions over a 30 minute period. A solution of 22.5 g of 2,3-dichloroanisole in 100 ml of 1,2-dichloroethane is added thereto. The mixture is stirred for one hour and poured over 100 ml concentrated HCl and ice. The organic layer is separated and the aqueous layer extracted with CHCl3. The organic extract is washed with water, dried (Na2SO4) and evaporated to give an oil which crystallizes from hexane to yield solid 2,3-dichloro-4-methoxy-2',6'-difluorobenzophenone which upon recrystallization from ether has an mp 94°-96° C.

Quelle