반응 #56546

ord-01d526c28d0343faaf6133d71910b692

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출extracted with ether
  2. 2
    건조The combined ether extracts are dried over magnesium sulfate
  3. 3
    여과filtered
  4. 4
    기타Into the ethereal solution is bubbled dry hydrogen chloride gas until no more oily precipitate forms
  5. 5
    기타The solvent is then decanted
  6. 6
    추출The purified free base is extracted into ether
  7. 7
    건조dried over magnesium sulfate
  8. 8
    기타When the solvent is evaporated

실험 절차

A mixture of 6-cyano-6-(2,4-dichlorophenyl)decyl bromide (14.2g., 0.036 mole) imidazole (10g., 0.15 mole) and 5 ml. N,N-dimethylformamide is heated at 120° C. for 24 hours. The reaction mixture is poured into water and extracted with ether. The combined ether extracts are dried over magnesium sulfate and filtered. Into the ethereal solution is bubbled dry hydrogen chloride gas until no more oily precipitate forms. The solvent is then decanted and the oily residue is taken up in acetone and neutralized with dilute ammonium hydroxide solution. The purified free base is extracted into ether and dried over magnesium sulfate. When the solvent is evaporated, a total of 6.5 g. (47.8%) of product is obtained, which is identified by nmr.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04225723uspto-grants-1980_09