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HCID 68157911、化合物 → 5-fluoro-N1-(2-fluorophenyl)benzene-1,2-diamine

HRID 243130
ノート
印刷プレビュー

反応式

HRID 243130 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 68157911HCID 68157911、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

(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)

後処理

  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
  • 出典と根拠

    ORDレコード
    ord-fd3cab791f594ed5adb0ecf400d19806
    出典データセット
    uspto-grants-2014_02
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US08653089B2

    反応ノート

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