Hydrazine hydrate (1:1) → 1,2-dihydro-6-nitro-3H-indazol-3-one

HRID 56612ノート

反応式

HRID 56612 の反応式
F[C:2]1[CH:11]=[C:10]([N+:12]([O-:14])=[O:13])[CH:9]=[CH:8][C:3]=1[C:4](OC)=[O:5].O.[NH2:16][NH2:17]>C(O)C.C(OCC)(=O)C>[N+:12]([C:10]1[CH:11]=[C:2]2[C:3]([C:4](=[O:5])[NH:16][NH:17]2)=[CH:8][CH:9]=1)([O-:14])=[O:13]

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 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 2

HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

In two portions of equal size, a total of 2.00 g (10.0 mmol) of methyl 2-fluoro-4-nitrobenzoate and 2.51 g (50.2 mmol) of hydrazine monohydrate in 36 ml of ethanol were heated in a microwave reactor at 120° C. for 2 h. The combined reaction solutions were diluted with ethyl acetate and washed with water. The aqueous phase was extracted three times with ethyl acetate. The combined organic phases were dried over magnesium sulphate and concentrated under reduced pressure. Yield: 1.66 g (purity 95%, 88% of theory)

後処理

  1. customThe combined reaction solutions
  2. washwashed with water
  3. extractionThe aqueous phase was extracted three times with ethyl acetate
  4. dry with materialThe combined organic phases were dried over magnesium sulphate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-bf55c5f94a744d7c8134953f9a135937
出典データセット
uspto-grants-2016_09
特許番号
US09434690B2

反応ノート

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