Ethanolamine → 2-(Bis(2-hydroxyethyl)amino)ethanesulphonic acid

HRID 128207

反応式

HRID 128207 の反応式
Br[CH:2]([S:4]([O-:7])(=[O:6])=[O:5])[CH3:3].[Na+].[CH2:9]([CH2:11][NH2:12])[OH:10].[CH2:13]([OH:15])[CH3:14]>O>[OH:10][CH2:9][CH2:11][N:12]([CH2:14][CH2:13][OH:15])[CH2:3][CH2:2][S:4]([OH:7])(=[O:6])=[O:5]

参加物

5

反応物 3

HCID 700EthanolamineHCID 702EthanolHCID 23705444Sodium bromoethanesulfonate

生成物 1

HCID 732432-(Bis(2-hydroxyethyl)amino)ethanesulphonic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-d1c4e63bcd184144bf099f58d9a8b652
出典データセット
uspto-grants-1981_03
特許番号
US04259332

関連ノート

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