반응 #2194

반응 방정식

Difluoromethyl chloride

4-chloro-4'-mercaptomethylbenzophenone

potassium hydroxide

dioxane

4-chloro-4'-mercaptomethylbenzophenone

→

desired product

수율 36.0%

4-Chloro-4'-difluoromethylthiomethyl-benzophenone

수율 36.0%

용매

water

반응 조건

후처리

1. 1
   여과subjected to filtration
2. 2
   건조The organic layer as the filtrate was dried over anhydrous magnesium sulfate
3. 3
   workup.ADDITIONadd
4. 4
   농축concentrated
5. 5
   기타The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=5:1)

실험 절차

4-chloro-4'-mercaptomethylbenzophenone (14.7 g) and potassium hydroxide (15 g) was added to a solvent comprising dioxane (100 ml) and water (100 ml). Difluoromethyl chloride was blown into this solution at 60° C. until the starting material 4-chloro-4'-mercaptomethylbenzophenone disappeared. The reaction product was cooled to room temperature and then subjected to filtration. The organic layer as the filtrate was dried over anhydrous magnesium sulfate add concentrated. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=5:1) to obtain the desired product (6.4 g, melting point: 34° to 35° C., yield: 36%).

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