Reaktion #2189

Reaktionsgleichung

4-chloro-4'-methylsulfonylmethylbenzophenone

hydrazine monohydrate

ethanol

→

desired product

Ausbeute 97.0%

4-Chloro-4'-methylsulfonylmethyl-benzophenone-hydrazone

Ausbeute 97.0%

Lösungsmittel

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturunder reflux
2. 2
   EinengenThe reaction mixture was concentrated
3. 3
   Extraktionthe residue 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
   SonstigeThe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1)

Vorschrift

4-chloro-4'-methylsulfonylmethylbenzophenone (10.0 g) and hydrazine monohydrate (4.9 g) were added to ethanol (200 ml) and acetic acid (10 ml), and the mixture was stirred for 6 hours under reflux. The reaction mixture was concentrated, and the residue 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 residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1) to obtain the desired product (10.0 g, melting point: 52° to 54° C., yield: 97%)

Quelle