Water → N-(3-aminophenyl)pentanamide

HRID 441276노트

반응식

HRID 441276 반응식
[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]

참가 물질

5

반응물 2

HCID 962WaterHCID 531778HCID 531778, 화합물

생성물 1

HCID 5138852N-(3-aminophenyl)pentanamide수율 98.3%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ca9d615e62c84de4b4aad95201a98513
출처 데이터셋
uspto-grants-1977_08
특허 번호
US04039316

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