Reaktion #1063715
ord-ff554c9e0c454383b80180a48ff08cfc
Reaktionsgleichung
Edukte
Reagenzien
Lösungsmittel
Reaktionsbedingungen
Aufarbeitung
- 1Temperaturwas refluxed for 3 hours
- 2TemperaturThe resulting mixture was further refluxed for 6 hours
- 3TemperaturThe reaction mixture was cooled
- 4Einengenconcentrated to about a half volume under reduced pressure
- 5workup.ADDITIONTo the concentrate were added 100 ml of ethyl acetate and 100 ml of water
- 6SonstigeThe organic layer was separated
- 7Waschenwashed with water
- 8Trocknena saturated aqueous sodium chloride solution in this order, and dried over anhydrous magnesium sulfate
- 9SonstigeThe solvent was removed by distillation under reduced pressure
- 10SonstigeTo the residue thus obtained
- 11FiltrationThe resulting crystals were collected by filtration
- 12Sonstigedried
Vorschrift
A mixture of 4.5 g of 1-(6-benzyloxy-2-naphthyl)-2-(2-chloroethoxy)ethanol, 1 g of potassium iodide, 10 ml of a 50% aqueous dimethylamine solution and 20 ml of ethanol was refluxed for 3 hours. To the reaction mixture was added 10 ml of a 50% aqueous dimethylamine solution. The resulting mixture was further refluxed for 6 hours. The reaction mixture was cooled and concentrated to about a half volume under reduced pressure. To the concentrate were added 100 ml of ethyl acetate and 100 ml of water. The mixture was adjusted to pH 10.5 with potassium carbonate. The organic layer was separated, washed with water and a saturated aqueous sodium chloride solution in this order, and dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure. To the residue thus obtained was added 30 ml of diethyl ether. The resulting crystals were collected by filtration and dried to obtain 3.9 g of 1-(6-benzyloxy-2-naphthyl)-2-[2-(N,N-dimethylamino)ethoxy]ethanol (compound No. 284).