تفاعل #2199

معادلة التفاعل

4-chloro-4'-trifluoromethylsulfonylmethylbenzophenone

Sodium borohydride

→

desired product

المردود 77.0%

4-Chloro-4'-trifluoromethylsulfonylmethylbenzhydrol

المردود 77.0%

المذيبات

methanol

methanol

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGthe mixture was further stirred overnight at room temperature
2. 2
   workup.DISTILLATIONwas distilled off under reduced pressure
3. 3
   استخلاصThe residue was extracted with ethyl acetate (250 ml)
4. 4
   غسيلThe extract was washed with water
5. 5
   تجفيفdried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONThen, ethyl 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'-trifluoromethylsulfonylmethylbenzophenone (5.5 g) was dispersed in methanol (200 ml). Sodium borohydride was gradually added thereto at room temperature with stirring, and the mixture was further stirred overnight at room temperature. After completion of the reaction, methanol was distilled off under reduced pressure. The residue was extracted with ethyl acetate (250 ml). The extract was washed with water and dried over anhydrous magnesium sulfate. Then, 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 as a white powder (4.2 g, melting point: 113° to 115° C., yield: 77%).

المصدر