反应 #2196

ord-27d91eecd20e450da1b8e17f791b0eaa

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONwas added to this solution
  2. 2
    浓缩The reaction mixture was concentrated
  3. 3
    workup.ADDITIONwater was added
  4. 4
    萃取The mixture was extracted with ethyl acetate
  5. 5
    洗涤The ethyl acetate layer was washed with water
  6. 6
    干燥dried over anhydrous magnesium sulfate
  7. 7
    workup.DISTILLATIONEthyl acetate was distilled off under reduced pressure
  8. 8
    洗涤The residual solid was washed with n-hexane

实验过程

4-chloro-4'-methylthiomethylbenzophenone (4.2 g) was added to methanol (150 ml). Sodium periodate (3.6 g) dissolved in water (20 ml), was added to this solution, and the mixture was stirred for 16 hours at room temperature. The reaction mixture was concentrated, and water was added thereto. The mixture was 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 (4.1 g, melting point: 116° to 118° C., yield: 93%).

来源

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