Reacción #2189

Ecuación de reacción

4-chloro-4'-methylsulfonylmethylbenzophenone

hydrazine monohydrate

ethanol

→

desired product

Rendimiento 97.0%

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

Rendimiento 97.0%

Disolventes

acetic acid

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturaunder reflux
2. 2
   ConcentraciónThe reaction mixture was concentrated
3. 3
   Extracciónthe residue was extracted with ethyl acetate
4. 4
   LavadoThe ethyl acetate layer was washed with water
5. 5
   Secadodried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONEthyl acetate was distilled off under reduced pressure
7. 7
   OtroThe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1)

Procedimiento

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%)

Fuente