Aminoacetaldehyde dimethyl acetal → HCID 3821256、化合物

HRID 1458021

反応式

HRID 1458021 の反応式
[CH3:1][O:2][CH:3]([O:6][CH3:7])[CH2:4][NH2:5].[S:8](Cl)([OH:11])(=O)=[O:9].[CH:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>C(=O)([O-])[O-].[Na+].[Na+]>[CH3:1][O:2][CH:3]([O:6][CH3:7])[CH2:4][NH:5][S:8]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)(=[O:11])=[O:9]

参加物

4

反応物 2

HCID 89728Aminoacetaldehyde dimethyl acetalHCID 22564087Benzene sulphochloride2 回

生成物 1

HCID 3821256HCID 3821256、化合物収率 101%

試薬・触媒・溶媒 1

HCID 10340Sodium Carbonate溶媒

実験手順

56 g 2-aminoacetaldehyde dimethyl acetal are dissolved in 200 ml of a 14 wt. % aqueous sodium carbonate solution at 20° C. in a three-necked flask, equipped with a thermometer, reflux condenser, tap funnel and magnetic stirrer. Subsequently, 88 g benzene sulfochloride are added drop-wise within 1 hour at this temperature under intensive stirring followed by another 2 hours of heating the reaction to 40° to 50° C. mixture under vigorous stirring. After that the intensive smell of benzene sulfochloride has disappeared and a second phase has formed. This heavy oily phase is separated in the separatory funnel, imbibed using diethyl ether and dried over water-free sodium sulfate. Once the drying agent has been removed and the ether has been distilled off, 112 g of the product are obtained (yield: 88% based on the amino acetal used).

後処理

  1. customequipped with a thermometer
  2. temperaturereflux condenser, tap funnel and magnetic stirrer
  3. temperatureof heating
  4. customthe reaction to 40° to 50° C. mixture under vigorous stirring
  5. customa second phase has formed
  6. customThis heavy oily phase is separated in the separatory funnel
  7. dry with materialdried over water-free sodium sulfate
  8. customOnce the drying agent has been removed
  9. distillationthe ether has been distilled off

出典と根拠

ORDレコード
ord-de843fe1380d4fdd9acd7e9e1dac6864
出典データセット
uspto-grants-1998_12
特許番号
US05849842

関連ノート

読み込み中…