Reaktion #2199

Reaktionsgleichung

4-chloro-4'-trifluoromethylsulfonylmethylbenzophenone

Sodium borohydride

→

desired product

Ausbeute 77.0%

4-Chloro-4'-trifluoromethylsulfonylmethylbenzhydrol

Ausbeute 77.0%

Lösungsmittel

methanol

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGthe mixture was further stirred overnight at room temperature
2. 2
   workup.DISTILLATIONwas distilled off under reduced pressure
3. 3
   ExtraktionThe residue was extracted with ethyl acetate (250 ml)
4. 4
   WaschenThe extract was washed with water
5. 5
   Trocknendried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONThen, ethyl acetate was distilled off under reduced pressure
7. 7
   SonstigeThe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1)

Vorschrift

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%).

Quelle