Reaktion #8336

ord-c51fe6fbce314d199d31f9750821f276

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe solution is refluxed for 12 h
  2. 2
    Einengenconcentrated in vacuo
  3. 3
    workup.ADDITIONThe residue is treated with dichloromethane/methanol
  4. 4
    Filtrationthe precipitate collected by vacuum filtration
  5. 5
    SonstigeThe precipitate is triturated with ethanol

Vorschrift

To a solution of (1-pyridin-2-yl-2-quinolin-4-yl-ethylidene)-hydrazine (2.0 g, 7.6 mmol) in pyridine (20 mL) at 0° C. is added ethyl chloroformate (2 mL) dropwise. The mixture is warmed to room temperature and stirred for 2 h. The solution is refluxed for 12 h and concentrated in vacuo. The residue is treated with dichloromethane/methanol and the precipitate collected by vacuum filtration. The precipitate is triturated with ethanol to yield the title compound, 300 mg (13%), as a white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07087626B2uspto-grants-2006_08