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HCID 68157911, 화합물 → 5-fluoro-N1-(2-fluorophenyl)benzene-1,2-diamine

HRID 243130
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HRID 243130 반응식
[F:1][C:2]1[CH:3]=[CH:4][C:5]([N+:16]([O-])=O)=[C:6]([NH:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[F:15])[CH:7]=1>CCOC(C)=O>[F:1][C:2]1[CH:7]=[C:6]([NH:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[F:15])[C:5]([NH2:16])=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 68157911HCID 68157911, 화합물

생성물 1

HCID 623760705-fluoro-N1-(2-fluorophenyl)benzene-1,2-diamine

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

(5-Fluoro-2-nitrophenyl)-(2-fluorophenyl)amine (3.04 g, 12.16 mmol) was dissolved in EtOAc (120 mL) and the flask evacuated and flushed with nitrogen gas. 10% Pd/C (0.3 g) was added and the reaction mixture stirred under an atmosphere of hydrogen gas, at RT overnight. A further amount of 10% Pd/C (0.3 g) was added and the reaction mixture stirred under an atmosphere of hydrogen gas for an extra 2 h. The resultant mixture was filtered through Celite® and the filtrate concentrated in vacuo to afford the title compound as a dark yellow oil, which solidified on standing (2.89 g, 95%). 1H NMR (CDCl3, 400 MHz): δ 7.05-6.87 (2H, m), 6.83-6.68 (3H, m), 6.68-6.59 (2H, m), 5.36 (1H, s), 3.49 (2H, s)

후처리

  1. custom
the flask evacuated
  • customflushed with nitrogen gas
  • addition10% Pd/C (0.3 g) was added
  • additionA further amount of 10% Pd/C (0.3 g) was added
  • stirringthe reaction mixture stirred under an atmosphere of hydrogen gas for an extra 2 h
  • filtrationThe resultant mixture was filtered through Celite®
  • concentrationthe filtrate concentrated in vacuo
  • 출처 및 근거

    ORD 기록
    ord-fd3cab791f594ed5adb0ecf400d19806
    출처 데이터셋
    uspto-grants-2014_02
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US08653089B2

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