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Ammonium Chloride → 1-(4-Amino-3-(trifluoromethyl)phenyl)ethanone

HRID 394865
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HRID 394865 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10](=[O:12])[CH3:11])=[CH:6][C:5]=1[C:13]([F:16])([F:15])[F:14])([O-])=O.[NH4+].[Cl-]>CCO.O.[Fe]>[NH2:1][C:4]1[CH:9]=[CH:8][C:7]([C:10](=[O:12])[CH3:11])=[CH:6][C:5]=1[C:13]([F:14])([F:15])[F:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 25517Ammonium ChlorideHCID 22313797HCID 22313797, 화합물

생성물 1

HCID 223138331-(4-Amino-3-(trifluoromethyl)phenyl)ethanone

시약·촉매·용매 3

HCID 23925Iron촉매HCID 702Ethanol용매HCID 962Water용매

실험 절차

A mixture of 1-[4-nitro-3-(trifluoromethyl)phenyl]-1-ethanone (1.41 g, 6.05 mmol), Fe powder (1.69 g, 30.2 mmol), and NH4Cl (324 mg, 6.05 mmol) in EtOH (24 ml) and water (9 ml) was heated to reflux for 2.5 hours. After cooling to room temperature, the mixture was filtered through a pad of Celite and the filtrate was concentrated. And the residue was dissolved with ethyl acetate (100 ml), washed with water (100 ml), dried over MgSO4, and concentrated in vacuo to give 1.22 g (quant.) of the title compound as a pale yellow oil.

후처리

  1. temperaturewas heated
  2. temperatureto reflux for 2.5 hours
  3. filtrationthe mixture was filtered through a pad of Celite
  4. concentrationthe filtrate was concentrated
  5. dissolutionAnd the residue was dissolved with ethyl acetate (100 ml)
  6. washwashed with water (100 ml)
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-313ee97aa9c742228677b3d48451b807
출처 데이터셋
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06603008B1

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