반응 #492115

ord-eee76d68c10244b0a17e46a5ab51c946

용매

반응 조건

온도
70°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타prepared
  2. 2
    workup.DISTILLATIONThe solvent was distilled off under vacuum, and hexane
  3. 3
    workup.ADDITIONwas added to the residue
  4. 4
    기타The insoluble matter was removed by filtration
  5. 5
    workup.DISTILLATIONthe solvent was thereafter distilled off under vacuum
  6. 6
    workup.DISTILLATIONThe resultant residue was distilled
  7. 7
    기타separated with an alumina column

실험 절차

In an argon atmosphere, 3.0 mL of 1,3-dimethylcyclopentadiene and 3.0 mL of ethylcyclopentadiene were added to a solution prepared by dissolving 0.51 g of ruthenium chloride hydrate in 40 mL of ethanol. Thereafter, 4.1 g of a zinc powder was added thereto. The mixture was stirred at 70° C. for 3 hours. The solvent was distilled off under vacuum, and hexane was added to the residue. The insoluble matter was removed by filtration, and the solvent was thereafter distilled off under vacuum. The resultant residue was distilled and then separated with an alumina column. Thus, 0.24 g of a yellow liquid was obtained (yield, 43%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08748644B2uspto-grants-2014_06