반응 #76414

ord-7395024a17624351a2345a5625fb037c

용매

반응 조건

온도
40°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타prepared
  2. 2
    추출extracted with ethyl acetate
  3. 3
    세척washed with water, brine
  4. 4
    건조dried over MgSO4
  5. 5
    기타evaporated
  6. 6
    기타The crude beige product is recrystallized from 130 ml of ethanol

실험 절차

A suspension of 4,4′-methanediyl-bis-benzenediazonium tetrafluoroborate (11.9 g, 0.03 mol), prepared according to the method of example 6.1, allyl cyanide (8.05 g; 0.12 mol), and palladium acetate (0.135 g, 0.6 mmol) in 80 ml of ethanol is heated at 40° C. during 22 h. The heterogeneous reaction mixture is poured into 300 ml of water, extracted with ethyl acetate, washed with water, brine, dried over MgSO4, and evaporated. The crude beige product is recrystallized from 130 ml of ethanol, yielding 5.44 g (61%) of 4-{4-[4-(3-cyano-propenyl)-benzyl]-phenyl}-but-3-enenitrile as light beige crystals, melting point 128-130° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06703182B1uspto-grants-2004_03