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

HRID 1041705노트

반응식

HRID 1041705 반응식
[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]

참가 물질

4

반응물 1

HCID 27833653,5-difluoro-2-nitrobenzoic acid

생성물 1

HCID 146519732-Amino-3,5-difluorobenzoic acid

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-9c33e11c1c774e119fd10bbf06bdd693
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08552186B2

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