반응 #2063061

ord-3cd5094adeef4f49b75cd011c0efecde

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도refluxed for one hour
  2. 2
    기타The solvent was evaporated
  3. 3
    기타the residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 95/5)
  4. 4
    기타The pure fractions were collected
  5. 5
    기타the solvent was evaporated
  6. 6
    workup.STIRRINGThe residue was stirred in diisopropylether/acetonitrile 10/1
  7. 7
    기타The solvent was evaporated

실험 절차

A mixture of 1-(3,4-dichlorophenyl)piperazine (0.1 mol), 2-propenenitrile (0.15 mol), and N-methyl-N,N-dioctyl octanaminiumchloride (1 ml) in 2-propanol (150 ml) was stirred and refluxed for one hour. The solvent was evaporated and the residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 95/5). The pure fractions were collected and the solvent was evaporated. The residue was stirred in diisopropylether/acetonitrile 10/1. The solvent was evaporated, yielding 28 g (98.5%) of 4-(3,4-dichlorophenyl)-1-piperazinepropanenitrile (intern. 3).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06224849B1uspto-grants-2001_05