反应 #2189

反应方程式

4-chloro-4'-methylsulfonylmethylbenzophenone

hydrazine monohydrate

ethanol

→

desired product

收率 97.0%

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

收率 97.0%

溶剂

acetic acid

反应条件

后处理

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

实验过程

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%)

来源