Реакция #2189

Уравнение реакции

4-chloro-4'-methylsulfonylmethylbenzophenone

hydrazine monohydrate

ethanol

→

desired product

Выход 97.0%

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

Выход 97.0%

Растворители

acetic acid

Условия реакции

Обработка

1. 1
   Температураunder reflux
2. 2
   КонцентрированиеThe reaction mixture was concentrated
3. 3
   Экстракцияthe residue was extracted with ethyl acetate
4. 4
   ПромывкаThe ethyl acetate layer was washed with water
5. 5
   Сушкаdried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONEthyl acetate was distilled off under reduced pressure
7. 7
   ДругоеThe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1)

Методика

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%)

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