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

HRID 56612노트

반응식

HRID 56612 반응식
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]

참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 3013872Methyl 2-fluoro-4-nitrobenzoate

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

실험 절차

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)

후처리

  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

출처 및 근거

ORD 기록
ord-bf55c5f94a744d7c8134953f9a135937
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09434690B2

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