반응 #82866

ord-cad2b301689e4acc8c686d1eb3ec0758

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooled in an ice bath
  2. 2
    기타After 5 hours the reaction was quenched with ice and ethylacetate and water
  3. 3
    workup.ADDITIONwere added
  4. 4
    기타The organic layer was seperated
  5. 5
    세척washed with water
  6. 6
    건조dried over MgSO4
  7. 7
    농축concentrated in vacuo
  8. 8
    기타The residue was recrystallized from dioxane and water

실험 절차

67.5 g (0.41 mol)3-acetamidoanisol are suspended in 200 ml 1,2-dichloroethane and cooled in an ice bath. 217 g (1.64 mol) AlCl3 and after it 38.5 g (0.49 mol) acetylchloride were added successively. Stirring was continued 1/2 hour. After 5 hours the reaction was quenched with ice and ethylacetate and water were added. The organic layer was seperated, washed with water, dried over MgSO4 and concentrated in vacuo. The residue was recrystallized from dioxane and water.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05622989uspto-grants-1997_04