Reaktion #416585
ord-82d4d90b35544a80aca467bfe97325ee
Reaktionsgleichung
Edukte
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1SonstigeTo a 125 ml round-bottomed flask equipped with condenser and N2 inlet
- 2TemperaturThe reaction was heated
- 3Temperaturat reflux for 5 days
- 4Temperaturcooled
- 5Filtrationthe precipitate filtered
- 6Waschenwashed with sodium bicarbonate
- 7Trocknendried over sodium sulfate
- 8workup.ADDITIONtreated with methylene chloride saturated with hydrochloride
- 9Sonstigeevaporated
- 10Sonstigethe residue triturated with ether
- 11Sonstigeto 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%).