Reaktion #2198

Reaktionsgleichung

4-bromomethyl-4'-chlorobenzophenone

sodium thiocyanate

ethanol

→

desired product

Ausbeute 42.0%

4-Chloro-4'-thiocyanatomethylbenzophenone

Ausbeute 42.0%

Lösungsmittel

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenThe reaction mixture was concentrated
2. 2
   workup.ADDITIONwater was added to the residue
3. 3
   ExtraktionThe mixture was extracted with ethyl acetate
4. 4
   WaschenThe ethyl acetate layer was washed with water
5. 5
   Trocknendried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONEthyl acetate was distilled off under reduced pressure
7. 7
   WaschenThe residual solid was washed with a solvent mixture of n-hexane

Vorschrift

4-bromomethyl-4'-chlorobenzophenone (5.7 g) and sodium thiocyanate (5.5 g) were added to ethanol (50 ml), and the mixture was stirred for one hour at 60° C. The reaction mixture was concentrated, and water was added to the residue. The mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with water and then dried over anhydrous magnesium sulfate. Ethyl acetate was distilled off under reduced pressure. The residual solid was washed with a solvent mixture of n-hexane:ethyl acetate=10:1 to obtain the desired product (2.2 g, melting point: 129° to 131° C., yield:42%).

Quelle