반응 #214421

ord-68c453afb2d64ef2b7b89777c2689575

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도under reflux
  2. 2
    온도to cool
  3. 3
    여과the inorganic residue was filtered off
  4. 4
    세척rinsed with acetone
  5. 5
    농축The filtrate was concentrated
  6. 6
    workup.DISTILLATIONby distilling off the solvent in vacuo
  7. 7
    기타The residue crystallized
  8. 8
    workup.ADDITIONafter the addition of 50 ml of diisopropyl ether

실험 절차

42.7 g (0.2 mol) of 1-bromo-4-chloro-3,3-dimethyl-butan-2-one were added dropwise to a boiling suspension of 41 g (0.2 mol) of 4-(4-chlorophenyl)-phenol and 28 g (0.2 mol) of potassium carbonate in 300 ml of absolute acetone. The mixture was stirred for 15 hours under reflux and was then allowed to cool and the inorganic residue was filtered off and rinsed with acetone. The filtrate was concentrated by distilling off the solvent in vacuo. The residue crystallized after the addition of 50 ml of diisopropyl ether. 37.5 g (55% of theory) of 4-chloro-1-[4-(4-chlorophenyl)-phenoxy]-3,3-dimethyl-butan-2-one of melting point 67°-68° C. were obtained.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04255434uspto-grants-1981_03