Reaktion #4459

ord-cc5f2343b0b2464494f03f96f151a07a

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter evaporation of chloroform
  2. 2
    Extraktionthe residue was extracted with ethyl acetate (100 ml)
  3. 3
    WaschenThe extract was washed with water
  4. 4
    Trocknendried over magnesium sulfate
  5. 5
    Sonstigeevaporated in vacuo
  6. 6
    SonstigeThe residue was chromatographed on silica gel (20 g)

Vorschrift

A solution of 4-fluoro-N-phenoxycarbonylaniline (2.29 g), N-amino-1,2,3,6-tetrahydropyridine hydrochloride (1.346 g) and triethylamine (1.02 g) in chloroform (25 ml) was refluxed for 20 hours. After evaporation of chloroform, the residue was extracted with ethyl acetate (100 ml). The extract was washed with water, dried over magnesium sulfate and evaporated in vacuo. The residue was chromatographed on silica gel (20 g) using chloroform as an eluent to give N-[[(4-fluorophenyl)carbamoyl]amino]-1,2,3,6-tetrahydropyridine (1.05 g). mp: 156°-157° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04725608uspto-grants-1988_02