Reaktion #215389

ord-d1c4e63bcd184144bf099f58d9a8b652

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.WAITthe reaction mixture left
  2. 2
    workup.WAITto stand for one night
  3. 3
    workup.DISTILLATIONThe excess diethanolamine and water were then distilled off under vacuum
  4. 4
    TemperaturThe solution was cooled
  5. 5
    Filtrationfiltered from the sodium chloride by a filter pump
  6. 6
    EinengenIt was then concentrated under vacuum until an oil
  7. 7
    Sonstigewas obtained which
  8. 8
    TemperaturOn cooling
  9. 9
    Sonstigea crystalline product was obtained
  10. 10
    Sonstigewas recrystallised from ethanol and water
  11. 11
    Sonstige16 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).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04259332uspto-grants-1981_03