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3-Nitro-5-(2-oxopyrrolidin-1-yl)benzoic acid → 3-Amino-5-(2-oxo-pyrrolidin-1-yl)-benzoic acid

HRID 852520
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반응식

HRID 852520 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([CH:10]=[C:11]([N:13]2[CH2:17][CH2:16][CH2:15][C:14]2=[O:18])[CH:12]=1)[C:7]([OH:9])=[O:8])([O-])=O>CO.O.[Pd]>[NH2:1][C:4]1[CH:5]=[C:6]([CH:10]=[C:11]([N:13]2[CH2:17][CH2:16][CH2:15][C:14]2=[O:18])[CH:12]=1)[C:7]([OH:9])=[O:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 222530233-Nitro-5-(2-oxopyrrolidin-1-yl)benzoic acid

생성물 1

HCID 222529903-Amino-5-(2-oxo-pyrrolidin-1-yl)-benzoic acid수율 95%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 22242641Methanol--water (1/1)용매

실험 절차

To a solution of 3-nitro-5-(2-oxo-pyrrolidin-1-yl)-benzoic acid (A27) (4 g, 16 mmol, 1 equiv) in MeOH/H2O (9:1, 40 ml) was added 10% palladium on charcoal (50% wet, 800 mg, 0.1 equiv w/w). The resulting mixture was stirred for 6 h at atmospheric pressure under an atmosphere of hydrogen. The catalyst was removed by filtration through a pad of celite and the solvent was removed in vacuo. The residue was dried at 60° C. under vacuum for 16 h to give 3-amino-5-(2-oxo-pyrrolidin-1-yl)-benzoic acid (D6) (3.34 g, 15.2 mmol, 95%) as a pale brown solid. [M−H]−=218.8, RT=1.86 min

후처리

  1. customThe catalyst was removed by filtration through a pad of celite
  2. customthe solvent was removed in vacuo
  3. customThe residue was dried at 60° C. under vacuum for 16 h

출처 및 근거

ORD 기록
ord-292d459d7c1149f3bde63c9cf17ace63
출처 데이터셋
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07253198B2

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