반응 #346765

ord-7257da434d7f4ae09948035558a99c5e

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The organic layer was separated
  2. 2
    추출The aqueous layer was extracted with methylene chloride
  3. 3
    세척the combined organic fractions were washed with water
  4. 4
    건조dried (magnesium sulphate)
  5. 5
    기타evaporated
  6. 6
    기타to yield a brown solid
  7. 7
    기타This was recrystallized from petroleum ether (60°-80°)

실험 절차

5-(4-Chlorobenzoyl)pentanoyl chloride (5.2g; 0.02 mole) in methylene chloride (100 ml) and ferrocene (3.75g; 0.02 mole) were stirred at 0.5° and aluminium chloride (2.7g; 0.02 mole) was added slowly over 0.5 hr. The mixture was stirred at 0.5° for 1.5 hr then water was added. The organic layer was separated. The aqueous layer was extracted with methylene chloride and the combined organic fractions were washed with water, dried (magnesium sulphate) and evaporated to yield a brown solid. This was recrystallized from petroleum ether (60°-80°) to yield pure 5-(4-chlorobenzoyl)pentanoyl ferrocene; 3.23g (40%); mp 103°-106°.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04038413uspto-grants-1977_07