Reaktion #416585

ord-82d4d90b35544a80aca467bfe97325ee

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeTo a 125 ml round-bottomed flask equipped with condenser and N2 inlet
  2. 2
    TemperaturThe reaction was heated
  3. 3
    Temperaturat reflux for 5 days
  4. 4
    Temperaturcooled
  5. 5
    Filtrationthe precipitate filtered
  6. 6
    Waschenwashed with sodium bicarbonate
  7. 7
    Trocknendried over sodium sulfate
  8. 8
    workup.ADDITIONtreated with methylene chloride saturated with hydrochloride
  9. 9
    Sonstigeevaporated
  10. 10
    Sonstigethe residue triturated with ether
  11. 11
    Sonstigeto afford a white solid, m.p. 305°-307° C., 1.76 g (48%)

Vorschrift

To a 125 ml round-bottomed flask equipped with condenser and N2 inlet were added 2.39 g (7.5 mmol) of 4-(4-(2-chloroethyl)phenyl)-2-methylthiazole hydrobromide, 1.59 g (7.5 mmol) of N-(1-naphthyl)piperazine, 1.31 ml (7.5 mmol) of diisopropylethylamine, 1.59 g (15 mmol) of sodium carbonate, 5 mg of sodium iodide, and 50 ml of methylisobutylketone. The reaction was heated at reflux for 5 days, cooled, and the precipitate filtered. The solid was taken up in methylene chloride, washed with sodium bicarbonate, dried over sodium sulfate, treated with methylene chloride saturated with hydrochloride, evaporated, and the residue triturated with ether to afford a white solid, m.p. 305°-307° C., 1.76 g (48%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04891375uspto-grants-1990_01