Réaction #2189

Équation de réaction

4-chloro-4'-methylsulfonylmethylbenzophenone

hydrazine monohydrate

ethanol

→

desired product

Rendement 97.0%

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

Rendement 97.0%

Solvants

acetic acid

Conditions de réaction

Traitement

1. 1
   Températureunder reflux
2. 2
   ConcentrationThe reaction mixture was concentrated
3. 3
   Extractionthe residue was extracted with ethyl acetate
4. 4
   LavageThe ethyl acetate layer was washed with water
5. 5
   Séchagedried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONEthyl acetate was distilled off under reduced pressure
7. 7
   AutreThe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1)

Mode opératoire

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%)

Source