반응 #54573

ord-99b41978505c4240bd53d8da44b02989

반응 조건

온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The solvent was removed under reduced pressure
  2. 2
    workup.ADDITIONthe resulting oil was poured into water
  3. 3
    추출The aqueous solution was extracted with ether
  4. 4
    건조the etheeal extracts were dried (MgSO4)
  5. 5
    기타evaporated under reduced pressure
  6. 6
    기타to yield an oil

실험 절차

Sodium hydride (0.93 g, 80% dispersion in oil) was added to a solution of 2,2-dimethyl-4-(3-trifluoromethylphenyl)chroman-7-ol (containing 1 mole of carbon tetrachloride of crystallisation) (7.5 g) in dimethylformamide (25 ml). Chloroacetonitrile (1.76 g) was added and the mixture heated at 60° C. for 3 hours. The solvent was removed under reduced pressure and the resulting oil was poured into water. The aqueous solution was extracted with ether and the etheeal extracts were dried (MgSO4) and evaporated under reduced pressure to yield an oil. Chromatography on alumina with ether--petrol (40°-60° C.); 1:3 as eluate gave the title compound which crystallised on standing.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04148909uspto-grants-1979_04