3,5-difluoro-2-nitrobenzoic acid → 2-Amino-3,5-difluorobenzoic acid

HRID 1041705ノート

反応式

HRID 1041705 の反応式
[F:1][C:2]1[C:3]([N+:12]([O-])=O)=[C:4]([CH:8]=[C:9]([F:11])[CH:10]=1)[C:5]([OH:7])=[O:6]>[Pd].CO>[NH2:12][C:3]1[C:2]([F:1])=[CH:10][C:9]([F:11])=[CH:8][C:4]=1[C:5]([OH:7])=[O:6]

参加物

4

反応物 1

HCID 27833653,5-difluoro-2-nitrobenzoic acid

生成物 1

HCID 146519732-Amino-3,5-difluorobenzoic acid

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

3,5-Difluoro-2-nitro-benzoic acid (2.908 g, 0.01432 mol), 10% Palladium on Carbon (50% Wet) (0.61 g). and Methanol (15 mL) was shaken under an atmosphere of Hydrogen at 38 PSI overnight. The reaction mixture was filtered through celite and concentrated under reduced pressure and azeotroped with toluene to give 2-Amino-3,5-difluoro-benzoic acid as off white solids (2.44 g, 99%). 1H-NMR (CDCl3): 7.45 (d, 1H, J=9.3 Hz), 7.03 (m, 1H), 5.65 (br s, 2H).

後処理

  1. filtrationThe reaction mixture was filtered through celite and
  2. concentrationconcentrated under reduced pressure
  3. customazeotroped with toluene

出典と根拠

ORDレコード
ord-9c33e11c1c774e119fd10bbf06bdd693
出典データセット
uspto-grants-2013_10
特許番号
US08552186B2

反応ノート

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