Diethyl Ether → 3-(2-Aminoethoxy)benzenamine

HRID 596601ノート

反応式

HRID 596601 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][CH:12]=1)[O:5][CH2:6][C:7]([NH2:9])=O.[H-].[Al+3].[Li+].[H-].[H-].[H-].CCOCC.[H-]>O>[NH2:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][CH:12]=1)[O:5][CH2:6][CH2:7][NH2:9]

参加物

6

反応物 4

HCID 3283Diethyl EtherHCID 166653HydrideHCID 104872522-(3-Aminophenoxy)acetamideHCID 21226445Aluminium lithium hydride

生成物 1

HCID 214503233-(2-Aminoethoxy)benzenamine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 3-aminophenoxyacetamide (10.0 g., 0.05 M), lithium aluminum hydride (6.8 g., 0.18 M) and ether (250 ml.) is refluxed under dry nitrogen for four days. It is then cooled to room temperature and water slowly added to decompose unreacted hydride. The precipitated salts are removed by filtration and the filtrate concentrated to an oil under reduced pressure. The crude oil is chromatographed on silica gel using 20% methanol/ethyl acetate as eluting agent. Concentration of appropriate fractions affords 4.83 g. (53%) of product as an oil. It is used without further purification.

後処理

  1. temperatureis refluxed under dry nitrogen for four days
  2. customThe precipitated salts are removed by filtration
  3. concentrationthe filtrate concentrated to an oil under reduced pressure
  4. customThe crude oil is chromatographed on silica gel using 20% methanol/ethyl acetate
  5. washas eluting agent
  6. customConcentration of appropriate fractions affords 4.83 g
  7. customIt is used without further purification

出典と根拠

ORDレコード
ord-ead4700b453b4c2db658b97fa9a81603
出典データセット
uspto-grants-1977_03
特許番号
US04011324

反応ノート

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