반응 #2195

ord-f13ed1df908340769124c76cde4ad555

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도under reflux
  2. 2
    농축The reaction mixture was concentrated
  3. 3
    추출extracted with ethyl acetate
  4. 4
    세척The ethyl acetate layer was washed with water
  5. 5
    건조dried over anhydrous magnesium sulfate
  6. 6
    workup.DISTILLATIONEthyl acetate was distilled off under reduced pressure
  7. 7
    세척The residual solid was washed with n-hexane

실험 절차

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%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05728699uspto-grants-1998_03