تفاعل #2189

معادلة التفاعل

4-chloro-4'-methylsulfonylmethylbenzophenone

hydrazine monohydrate

ethanol

→

desired product

المردود 97.0%

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

المردود 97.0%

المذيبات

acetic acid

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةunder reflux
2. 2
   تركيزThe reaction mixture was concentrated
3. 3
   استخلاصthe residue was extracted with ethyl acetate
4. 4
   غسيلThe ethyl acetate layer was washed with water
5. 5
   تجفيفdried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONEthyl acetate was distilled off under reduced pressure
7. 7
   أخرىThe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1)

الإجراء التجريبي

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%)

المصدر