Hydrazine → 1,2-dihydro-6-nitro-3H-indazol-3-one

HRID 1176022노트

반응식

HRID 1176022 반응식
C[O:2][C:3](=O)[C:4]1[CH:9]=[CH:8][C:7]([N+:10]([O-:12])=[O:11])=[CH:6][C:5]=1F.[NH2:15][NH2:16]>C(O)C>[N+:10]([C:7]1[CH:6]=[C:5]2[C:4]([C:3](=[O:2])[NH:15][NH:16]2)=[CH:9][CH:8]=1)([O-:12])=[O:11]

참가 물질

4

반응물 2

HCID 9321HydrazineHCID 3013872Methyl 2-fluoro-4-nitrobenzoate

생성물 1

HCID 32644791,2-dihydro-6-nitro-3H-indazol-3-one

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

The crude material, 2-fluoro-4-nitro-benzoic acid methyl ester, from above was treated with hydrazine (1.6 mL, 51 mmol) in ethanol under reflux for 14 hrs. After removal of solvent by evaporation, the residue was washed with water. The precipitate product was filtered and dried on the vacuum pump to give the title compound which was used without further purification (4.0 g, 85% for two steps). MS (ES+): m/e=180.1 (M+H), 178.0 (M-H); LC/Method A 1.83 min.

후처리

  1. temperatureunder reflux for 14 hrs
  2. customAfter removal of solvent
  3. customby evaporation
  4. washthe residue was washed with water
  5. filtrationThe precipitate product was filtered
  6. customdried on the vacuum pump

출처 및 근거

ORD 기록
ord-eeb45d2046d84206b9d86b8d6fdf86ab
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07842712B2

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