Ethylenediamine → N-(2-aminoethyl)thiophene-2-carboxamide

HRID 1589199

反応式

HRID 1589199 の反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]([O:8]CC)=O.[CH2:11]([NH2:14])[CH2:12][NH2:13]>C1(C)C=CC=CC=1>[NH2:13][CH2:12][CH2:11][NH:14][C:6]([C:2]1[S:1][CH:5]=[CH:4][CH:3]=1)=[O:8]

参加物

4

反応物 2

HCID 3301EthylenediamineHCID 76052Ethyl 2-thenoate

生成物 1

HCID 4649097N-(2-aminoethyl)thiophene-2-carboxamide

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
97.5 °C

実験手順

A mixture of ethyl thiophene-2-carboxylate (12.0 g.) and ethylenediamine (15.4 ml.) was heated at 95-100° C. for 48 hours. Excess ethylenediamine was removed under reduced pressure and the residue was dissolved in water (150 ml.). The insoluble material [bis(carboxamide)derivative] was removed by filtration. Evaporation of the filtrate gave a residue which was dissolved in toluene (50 ml.). The mixture was evaporated to give N-(2-aminoethyl)-thiophene-2-carboxamide as an oil (12.0 g.) essentially pure by TLC (Rf 0.90; Si02 : 10% v/v methanol in chloroform as eluant) which was used without purification.

後処理

  1. customExcess ethylenediamine was removed under reduced pressure
  2. dissolutionthe residue was dissolved in water (150 ml.)
  3. customThe insoluble material [bis(carboxamide)derivative] was removed by filtration
  4. customEvaporation of the filtrate
  5. customgave a residue which
  6. customThe mixture was evaporated

出典と根拠

ORDレコード
ord-75d163724c0846ce93ba2bd13c47c536
出典データセット
uspto-grants-1986_02
特許番号
US04568691

関連ノート

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