反応 #2199

反応方程式

4-chloro-4'-trifluoromethylsulfonylmethylbenzophenone

Sodium borohydride

→

desired product

収率 77.0%

4-Chloro-4'-trifluoromethylsulfonylmethylbenzhydrol

収率 77.0%

溶媒

methanol

methanol

反応条件

後処理

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

実験手順

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%).

出典