反应 #2195

ord-f13ed1df908340769124c76cde4ad555

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05728699uspto-grants-1998_03