反应 #54573

ord-99b41978505c4240bd53d8da44b02989

反应条件

温度
60°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The solvent was removed under reduced pressure
  2. 2
    workup.ADDITIONthe resulting oil was poured into water
  3. 3
    萃取The aqueous solution was extracted with ether
  4. 4
    干燥the etheeal extracts were dried (MgSO4)
  5. 5
    其他evaporated under reduced pressure
  6. 6
    其他to yield an oil

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04148909uspto-grants-1979_04