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

HRID 855637ノート

反応式

HRID 855637 の反応式
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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d064b788bb014970b2a85ae9f1b5d0b2
出典データセット
uspto-grants-2007_08
特許番号
US07262200B2

反応ノート

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