o-Phenetidine → N-glycidyl-2-ethoxyaniline

HRID 437193

反応式

HRID 437193 の反応式
[CH2:1]([O:3][C:4]1[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=1[NH2:6])[CH3:2].[CH2:11]([CH:13]1[O:15][CH2:14]1)Cl>CO>[CH2:11]([NH:6][C:5]1[CH:7]=[CH:8][CH:9]=[CH:10][C:4]=1[O:3][CH2:1][CH3:2])[CH:13]1[O:15][CH2:14]1

参加物

4

反応物 2

HCID 7203o-PhenetidineHCID 7835Epichlorohydrin

生成物 1

HCID 21430375N-glycidyl-2-ethoxyaniline

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
25 °C

実験手順

A mixture of 2-ethoxyaniline (54.8 g.), methanol (300 ml.) and epichlorhydrin (18.6 g.) is stirred at 25° C. for 24 hours. The methanol and unreacted 2-ethoxyaniline are removed by vacuum distillation and the residue is dissolved in methanol (300 ml.) and sodium hydroxide (8.0 g.) added. The mixture is stirred at 25° C. for 3 hours, filtered and the filtrate evaporated under reduced pressure to give N-glycidyl-2-ethoxyaniline which is then dissolved in methanol (69 ml.). This solution is added to a stirred suspension of 2-aminoethyl hydrogen sulphate (97.0 g.) in a mixture of methanol (69 ml.), water (16.5 ml.) and sodium hydroxide solution (17 N; 35.0 ml.). The mixture is stirred at 25° C. for 16 hours.

後処理

  1. customThe methanol and unreacted 2-ethoxyaniline are removed by vacuum distillation
  2. dissolutionthe residue is dissolved in methanol (300 ml.)
  3. additionsodium hydroxide (8.0 g.) added
  4. stirringThe mixture is stirred at 25° C. for 3 hours
  5. filtrationfiltered
  6. customthe filtrate evaporated under reduced pressure

出典と根拠

ORDレコード
ord-c88b1eaddd2e4553990d31a09f8aa47c
出典データセット
uspto-grants-1977_06
特許番号
US04029786

関連ノート

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