5-fluoro-N-methyl-2-nitroaniline → 5-Fluoro-N1-methylbenzene-1,2-diamine

HRID 1048937ノート

反応式

HRID 1048937 の反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]([N+:10]([O-])=O)=[C:6]([CH:9]=1)[NH:7][CH3:8]>[Pd].CO>[F:1][C:2]1[CH:9]=[C:6]([NH:7][CH3:8])[C:5]([NH2:10])=[CH:4][CH:3]=1

参加物

4

反応物 1

HCID 229057745-fluoro-N-methyl-2-nitroaniline

生成物 1

HCID 184572835-Fluoro-N1-methylbenzene-1,2-diamine

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

To the title compound from Example 1 Step A (0.267 g, 1.57 mmol) were added palladium on carbon (0.027 g) and methanol (7.85 mL). The resulting mixture was stirred under an atmosphere of hydrogen at room temperature overnight. The mixture was then filtered through CELITE® using dichloromethane, and the filtrate was concentrated. Purification by flash chromatography (50% ethyl acetate in hexanes, then 100% ethyl acetate) provided the title compound: 1H NMR (500 MHz, CDCl3) δ 6.61 (dd, J=8.2, 5.6 Hz, 1 H), 6.36-6.30 (m, 2 H), 3.22 (br s, 3 H), 2.84 (s, 3 H).

後処理

  1. filtrationThe mixture was then filtered through CELITE®
  2. concentrationthe filtrate was concentrated
  3. customPurification by flash chromatography (50% ethyl acetate in hexanes

出典と根拠

ORDレコード
ord-33b884d3682748a2a1cef0f56413be90
出典データセット
uspto-grants-2016_07
特許番号
US09382226B2

反応ノート

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