反応 #82254

反応方程式

2-acetyl-5-benzofurancarbonitrile

bromine

chloroform

→

2-(2-bromo-1-oxoethyl)-5-benzofurancarbonitrile

収率 70.1%

溶媒

dichloromethane

dichloromethane

反応条件

後処理

1. 1
   workup.ADDITIONwas added dropwise to the above solution
2. 2
   温度After gradually warming up to ice-cold temperature
3. 3
   その他the resulting reaction solution
4. 4
   洗浄washed with 10% sodium thiosulfate aqueous solution
5. 5
   その他After drying
6. 6
   濃縮the organic layer and subsequent concentration to dryness
7. 7
   その他the resulting residue was recrystallized from a benzene/n-hexane mixture

実験手順

21.0 g of 2-acetyl-5-benzofurancarbonitrile was dissolved in 300 ml of dichloromethane. With stirring at a temperature of -10° C., 30 ml of dichloromethane solution containing 18.2 g of bromine was added dropwise to the above solution. After gradually warming up to ice-cold temperature, the resulting reaction solution was mixed with chloroform and washed with 10% sodium thiosulfate aqueous solution. After drying the organic layer and subsequent concentration to dryness, the resulting residue was recrystallized from a benzene/n-hexane mixture to obtain 21.0 g of 2-(2-bromo-1-oxoethyl)-5-benzofurancarbonitrile in the form of colorless crystals.

出典