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4-nitro-1H-pyrazole-3-carboxylic acid (2-amino-4,5-dimethoxy-phenyl)-amide → 5,6-Dimethoxy-2-(4-nitro-1,2-dihydro-3H-pyrazol-3-ylidene)-2H-benzimidazole

HRID 1012144
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HRID 1012144 반응식
[NH2:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[C:5]([O:10][CH3:11])=[CH:4][C:3]=1[NH:12][C:13]([C:15]1[C:19]([N+:20]([O-:22])=[O:21])=[CH:18][NH:17][N:16]=1)=O>C(O)(=O)C>[CH3:11][O:10][C:5]1[C:6]([O:8][CH3:9])=[CH:7][C:2]2[NH:1][C:13]([C:15]3[C:19]([N+:20]([O-:22])=[O:21])=[CH:18][NH:17][N:16]=3)=[N:12][C:3]=2[CH:4]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 1784932234-nitro-1H-pyrazole-3-carboxylic acid (2-amino-4,5-dimethoxy-phenyl)-amide

생성물 1

HCID 1784867955,6-Dimethoxy-2-(4-nitro-1,2-dihydro-3H-pyrazol-3-ylidene)-2H-benzimidazole수율 94%

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
140 °C

실험 절차

4-Nitro-1H-pyrazole-3-carboxylic acid (2-amino-4,5-dimethoxy-phenyl)-amide (2.35 g, 7.65 mmol) was dissolved in acetic acid (150 ml) and refluxed at 140° C. for 5 hours. The solution was left to cool and the solvent removed in vacuo. The resulting solid was partitioned between ethyl acetate (25 ml) and brine (25 ml). The organic layer was separated, dried (MgSO4), filtered and the solvent removed in vacuo to yield 5,6-dimethoxy-2-(4-nitro-1H-pyrazol-3-yl)-1H-benzimidazole (2.08 g, 94%).

후처리

  1. waitThe solution was left
  2. temperatureto cool
  3. customthe solvent removed in vacuo
  4. customThe resulting solid was partitioned between ethyl acetate (25 ml) and brine (25 ml)
  5. customThe organic layer was separated
  6. dry with materialdried (MgSO4)
  7. filtrationfiltered
  8. customthe solvent removed in vacuo

출처 및 근거

ORD 기록
ord-818dabe71927476091df741f37588387
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07977477B2

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