Reaktion #655867

Reaktionsgleichung

HCl

AlCl3

2,3-dichloroanisole

o-methoxybenzoyl chloride

→

2,3-dichloro-2',4-dimethoxybenzophenone

Lösungsmittel

1,2-dichloroethane

hexane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGThe mixture is stirred one half hour
2. 2
   ExtraktionThe aqueous layer is extracted with additional organic solvent
3. 3
   WaschenThe combined organic layers are washed until neutral,
4. 4
   Trocknendried over Na2SO4
5. 5
   Sonstigeevaporated
6. 6
   Sonstigeto give an oil which
7. 7
   SonstigeThe crude product is recrystallized from 95% ethanol

Vorschrift

To a mixture of 3.9 g of AlCl3 and 4.67 g of 2,3-dichloroanisole in 70 ml of 1,2-dichloroethane at -10° C., 5 g of o-methoxybenzoyl chloride is added dropwise. The mixture is stirred for 2.5 hours and is gradually warmed to 5° C. The reaction mixture is poured into concentrated HCl and ice. The mixture is stirred one half hour to decompose the complex. The aqueous layer is extracted with additional organic solvent. The combined organic layers are washed until neutral, dried over Na2SO4 and evaporated to give an oil which solidifies on trituration with hexane. The crude product is recrystallized from 95% ethanol giving 2,3-dichloro-2',4-dimethoxybenzophenone, mp 94°-96° C.

Quelle