Реакция #56546

ord-01d526c28d0343faaf6133d71910b692

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Экстракцияextracted with ether
  2. 2
    СушкаThe combined ether extracts are dried over magnesium sulfate
  3. 3
    Фильтрацияfiltered
  4. 4
    ДругоеInto the ethereal solution is bubbled dry hydrogen chloride gas until no more oily precipitate forms
  5. 5
    ДругоеThe solvent is then decanted
  6. 6
    ЭкстракцияThe purified free base is extracted into ether
  7. 7
    Сушкаdried over magnesium sulfate
  8. 8
    ДругоеWhen the solvent is evaporated

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04225723uspto-grants-1980_09