Ammonium Chloride → 1-(3-Amino-4-Methylphenyl)Ethanone

HRID 1712891

반응식

HRID 1712891 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:10])[CH3:9])=[CH:4][C:3]=1[N+:11]([O-])=O.[NH4+].[Cl-]>C(O)C.O.[Fe]>[NH2:11][C:3]1[CH:4]=[C:5]([C:8](=[O:10])[CH3:9])[CH:6]=[CH:7][C:2]=1[CH3:1]

참가 물질

6

반응물 2

HCID 25517Ammonium ChlorideHCID 792463'-Nitro-4'-methylacetophenone

생성물 1

HCID 3429141-(3-Amino-4-Methylphenyl)Ethanone수율 89.4%

시약·촉매·용매 3

HCID 23925Iron촉매HCID 702Ethanol용매HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

A mixture of 1-(4-methyl-3-nitrophenyl)ethanone (5.37 g, 30 mmol), iron powder (8.4 g, 150 mmol) and NH4Cl (1.62 g, 30 mmol) in ethanol (100 mL) and water (10 mL) was heated at 80° C. overnight. The mixture was then heated at 110° C. for 5 hours and allowed to cool to room temperature. The resulting suspension was filtered and the filter cake was washed with ethanol. The filtrate was concentrated and the residue was dissolved in ethanol and filtered. The filtrate was concentrated to give 4 g of the title compound as a yellow solid. MS(ESI(+)) m/e 149.8 (M+H)+.

후처리

  1. temperatureThe mixture was then heated at 110° C. for 5 hours
  2. temperatureto cool to room temperature
  3. filtrationThe resulting suspension was filtered
  4. washthe filter cake was washed with ethanol
  5. concentrationThe filtrate was concentrated
  6. dissolutionthe residue was dissolved in ethanol
  7. filtrationfiltered
  8. concentrationThe filtrate was concentrated

출처 및 근거

ORD 기록
ord-102a050088294d7da144636186144569
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07795248B2

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