반응 #2197

반응 방정식

4-(3-bromopropyl)sulfonylmethyl-4'-chlorobenzophenone

sodium hydride

N,N-dimethylacetamide

→

desired product

수율 50.0%

4-Chloro-4'-(1,1-dioxothiolan-2-yl)benzophenone

수율 50.0%

용매

Water

반응 조건

후처리

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

실험 절차

4-(3-bromopropyl)sulfonylmethyl-4'-chlorobenzophenone (2.5 g) and 60% sodium hydride (0.3 g) were added to N,N-dimethylacetamide (70 ml), and the mixture was stirred for 16 hours at room temperature. Water was added to the reaction mixture, and 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 residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=1:1) to obtain the desired product as a slightly yellow viscous substance 1.0 g, yield: 50%).

출처