Реакция #2197

Уравнение реакции

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

sodium hydride

N,N-dimethylacetamide

→

desired product

Выход 50.0%

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

Выход 50.0%

Растворители

Water

Условия реакции

Обработка

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

Методика

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%).

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