反応 #2195

反応方程式

4-bromomethyl-4'-chlorobenzophenone

methylmercaptan sodium

→

desired product

収率 83.0%

4-Chloro-4'-methylthiomethylbenzophenone

収率 83.0%

溶媒

methanol

反応条件

後処理

1. 1
   温度under reflux
2. 2
   濃縮The reaction mixture was concentrated
3. 3
   抽出extracted with ethyl acetate
4. 4
   洗浄The ethyl acetate layer was washed with water
5. 5
   乾燥dried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONEthyl acetate was distilled off under reduced pressure
7. 7
   洗浄The residual solid was washed with n-hexane

実験手順

4-bromomethyl-4'-chlorobenzophenone (3.1 g) and 15% methylmercaptan-sodium aqueous solution (5.6 g) were added to methanol (150 ml), and the mixture was stirred for 30 minutes under reflux. The reaction mixture was concentrated and extracted with ethyl acetate. The ethyl acetate layer was washed with water and then dried over anhydrous magnesium sulfate. Ethyl acetate was distilled off under reduced pressure. The residual solid was washed with n-hexane to obtain the desired product (2.3 g, melting point: 59° to 61° C., yield: 83%).

出典