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

HRID 1688047노트

반응식

HRID 1688047 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-40d82ba75da24319a6ed4afa8daa79cf
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08148391B2

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