反応 #2189

反応方程式

4-chloro-4'-methylsulfonylmethylbenzophenone

hydrazine monohydrate

ethanol

→

desired product

収率 97.0%

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

収率 97.0%

溶媒

acetic acid

反応条件

後処理

1. 1
   温度under reflux
2. 2
   濃縮The reaction mixture was concentrated
3. 3
   抽出the residue was extracted with ethyl acetate
4. 4
   洗浄The ethyl acetate layer was washed with water
5. 5
   乾燥dried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONEthyl acetate was distilled off under reduced pressure
7. 7
   その他The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1)

実験手順

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%)

出典