Hydrochloric Acid → 4-Nitro-1,2-dihydro-3H-indazol-3-one

HRID 2112076노트

반응식

HRID 2112076 반응식
[NH2:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([N+:11]([O-:13])=[O:12])[C:3]=1[C:4](O)=[O:5].Cl.[N:15]([O-])=O.[Na+].S(=O)=O>O>[N+:11]([C:7]1[CH:8]=[CH:9][CH:10]=[C:2]2[C:3]=1[C:4](=[O:5])[NH:15][NH:1]2)([O-:13])=[O:12]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 1119Sulfur Dioxide2회HCID 957952-Amino-6-nitro-benzoic acidHCID 23668193Sodium Nitrite

생성물 1

HCID 247281924-Nitro-1,2-dihydro-3H-indazol-3-one

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

5 g (27.5 mmol) 2-amino-6-nitro-benzoic acid are combined with 22.2 ml (225.3 mmol) concentrated HCl and 45 ml (30.0 mmol) 5% aqueous sodium nitrite solution and stirred for 1 h at ambient temperature. Then the suspension is diluted with 150 ml dist. H2O and added dropwise to 350 ml destilliertes water which has been saturated with sulphur dioxide. Sulphur dioxide is piped through the reaction mixture for a further 30 min. Then the reaction mixture is refluxed for 30 min and then left to cool slowly to 20° C. The resulting precipitate is filtered off.

후처리

  1. additionThen the suspension is diluted with 150 ml dist
  2. temperatureThen the reaction mixture is refluxed for 30 min
  3. waitleft
  4. temperatureto cool slowly to 20° C
  5. filtrationThe resulting precipitate is filtered off

출처 및 근거

ORD 기록
ord-d327fcefa8d440e79300a236590609fb
출처 데이터셋
uspto-grants-2009_04
특허 번호
US07521457B2

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