반응 #2189

반응 방정식

4-chloro-4'-methylsulfonylmethylbenzophenone

hydrazine monohydrate

ethanol

→

desired product

수율 97.0%

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

수율 97.0%

용매

acetic acid

반응 조건

후처리

1. 1
   온도under reflux
2. 2
   농축The reaction mixture was concentrated
3. 3
   추출the residue was extracted with ethyl acetate
4. 4
   세척The ethyl acetate layer was washed with water
5. 5
   건조dried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONEthyl acetate was distilled off under reduced pressure
7. 7
   기타The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1)

실험 절차

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%)

출처