Reaktion #215389
ord-d1c4e63bcd184144bf099f58d9a8b652
Reagenzien
Lösungsmittel
Reaktionsbedingungen
Aufarbeitung
- 1workup.WAITthe reaction mixture left
- 2workup.WAITto stand for one night
- 3workup.DISTILLATIONThe excess diethanolamine and water were then distilled off under vacuum
- 4TemperaturThe solution was cooled
- 5Filtrationfiltered from the sodium chloride by a filter pump
- 6EinengenIt was then concentrated under vacuum until an oil
- 7Sonstigewas obtained which
- 8TemperaturOn cooling
- 9Sonstigea crystalline product was obtained
- 10Sonstigewas recrystallised from ethanol and water
- 11Sonstige16 G of product were obtained
Vorschrift
A solution of 90 g of sodium bromoethanesulphonate (Organic Synthesis, Coll. Vol. II, p; 558) and 110 g of ethanolamine in 1500 ml of water was heated over a steam bath for about 2 hours and the reaction mixture left to stand for one night. The excess diethanolamine and water were then distilled off under vacuum, and the residue taken up in 100 ml of water and 800 ml of concentrated hydrochloric acid. The solution was cooled and filtered from the sodium chloride by a filter pump. It was then concentrated under vacuum until an oil was obtained which was taken up in boiling ethanol. On cooling, a crystalline product was obtained having a melting point of 163°-165° C., which was recrystallised from ethanol and water. 16 G of product were obtained, the analytical and spectroscopic data of which confirmed the identity of the product as the compound (III).