Реакция #2199

Уравнение реакции

4-chloro-4'-trifluoromethylsulfonylmethylbenzophenone

Sodium borohydride

→

desired product

Выход 77.0%

4-Chloro-4'-trifluoromethylsulfonylmethylbenzhydrol

Выход 77.0%

Растворители

methanol

methanol

Условия реакции

Обработка

1. 1
   workup.STIRRINGthe mixture was further stirred overnight at room temperature
2. 2
   workup.DISTILLATIONwas distilled off under reduced pressure
3. 3
   ЭкстракцияThe residue was extracted with ethyl acetate (250 ml)
4. 4
   ПромывкаThe extract was washed with water
5. 5
   Сушкаdried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONThen, ethyl 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'-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%).

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