5-Hydroxy-4-methoxy-2-nitrobenzoic acid → 2-Amino-5-hydroxy-4-methoxybenzoic acid

HRID 1725139노트

반응식

HRID 1725139 반응식
[OH:1][C:2]1[C:3]([O:14][CH3:15])=[CH:4][C:5]([N+:11]([O-])=O)=[C:6]([CH:10]=1)[C:7]([OH:9])=[O:8]>CO.O=[Pt]=O>[NH2:11][C:5]1[CH:4]=[C:3]([O:14][CH3:15])[C:2]([OH:1])=[CH:10][C:6]=1[C:7]([OH:9])=[O:8]

참가 물질

4

반응물 1

HCID 139156695-Hydroxy-4-methoxy-2-nitrobenzoic acid

생성물 1

HCID 198070282-Amino-5-hydroxy-4-methoxybenzoic acid수율 97.4%

시약·촉매·용매 2

HCID 345198Adams' catalyst촉매HCID 887Methanol용매

실험 절차

5-Hydroxy-4-methoxy-2-nitro-benzoic acid (18 g, 84.51 mmol, J. Indian Chem. Soc. 1970, 70, 925) is suspended in MeOH (1 L) and treated PtO2 (100 mg). The flask is flushed with hydrogen gas and the reaction mixture is stirred under hydrogen atmosphere (45 psi) for 4 hours. The reaction mixture is filtered through a celite plug and the solvent is removed under reduced pressure. The crude product is redissolved in DCM, dried (MgSO4) and concentrated to yield 15.06 g (82.3 mmol, 97%) of the desired product.

후처리

  1. customThe flask is flushed with hydrogen gas
  2. filtrationThe reaction mixture is filtered through a celite plug
  3. customthe solvent is removed under reduced pressure
  4. dissolutionThe crude product is redissolved in DCM
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-7ed3eaf8f03047b997400c18b1702cbb
출처 데이터셋
uspto-grants-2009_02
특허 번호
US07488823B2

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