반응 #63977

ord-6f8933fba88e466eb7e9c768e979dc7a

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the mixture heated
  2. 2
    온도under reflux for eighteen hours
  3. 3
    온도The mixture was cooled
  4. 4
    workup.STIRRINGThe resulting mixture was stirred
  5. 5
    온도under reflux for ten hours
  6. 6
    추출extracted with ether
  7. 7
    추출The ether extract

실험 절차

1-(4-Chlorophenyl)-1-cyclobutanecarbonitrile (15 g) prepared in a similar manner to the 1-(3,4-dichlorophenyl)cyclobutanecarbonitrile of Example 1 in dry ether (50 ml) was added to the product of the reaction between magnesium turnings (3.18 g) and propyl bromide (15.99 g) in dry ether (50 ml). The ether was replaced by tetrahydrofuran and the mixture heated with stirring under reflux for eighteen hours. The mixture was cooled and ice and then concentrated hydrochloric acid (52 ml) added. The resulting mixture was stirred under reflux for ten hours and extracted with ether. The ether extract yielded a residue from which 1-butyryl-1-(4-chlorophenyl)cyclobutane (b.p. 106°-108°/0.3 mm Hg) was distilled.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04767790uspto-grants-1988_08