HRID128207

反应详情

EQUATION

反应方程式

HRID 128207 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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).

WORKUP

后处理

  1. waitthe reaction mixture left
  2. waitto stand for one night
  3. distillationThe excess diethanolamine and water were then distilled off under vacuum
  4. temperatureThe solution was cooled
  5. filtrationfiltered from the sodium chloride by a filter pump
  6. concentrationIt was then concentrated under vacuum until an oil
  7. customwas obtained which
  8. temperatureOn cooling
  9. customa crystalline product was obtained
  10. customwas recrystallised from ethanol and water
  11. custom16 G of product were obtained