Water → N-(3-aminophenyl)pentanamide

HRID 441276ノート

反応式

HRID 441276 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([CH:14]=[CH:15][CH:16]=1)[NH:7][C:8](=[O:13])[CH2:9][CH2:10][CH2:11][CH3:12])([O-])=O.O>[Fe].C(O)C>[NH2:1][C:4]1[CH:5]=[C:6]([CH:14]=[CH:15][CH:16]=1)[NH:7][C:8](=[O:13])[CH2:9][CH2:10][CH2:11][CH3:12]

参加物

5

反応物 2

HCID 962WaterHCID 531778HCID 531778、化合物

生成物 1

HCID 5138852N-(3-aminophenyl)pentanamide収率 98.3%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 702Ethanol溶媒

実験手順

A mixture of 177.6 g of m-nitrovaleranilide, 160 ml of water, 8 ml of 22° Be hydrochloric acid and 640 ml of 95% ethanol was refluxed and 480 g of iron powder were added with stirring over 30 minutes. Reflux was continued for 30 minutes with stirring and the mixture was filtered. The filtrate was concentrated to dryness under reduced pressure and the residue was chromatographed over silica gel. Elution with an 8- 2 methylene chloride-acetone mixture gave 151 g of m-aminovaleranilide with a specific rotation nD20 = 1.541.

後処理

  1. temperaturewas refluxed
  2. temperatureReflux
  3. waitwas continued for 30 minutes
  4. stirringwith stirring
  5. filtrationthe mixture was filtered
  6. concentrationThe filtrate was concentrated to dryness under reduced pressure
  7. customthe residue was chromatographed over silica gel
  8. washElution with an 8- 2 methylene chloride-acetone mixture

出典と根拠

ORDレコード
ord-ca9d615e62c84de4b4aad95201a98513
出典データセット
uspto-grants-1977_08
特許番号
US04039316

反応ノート

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