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1,1-Dimethylhydrazine monohydrochloride → 1,3-Dimethyl-5-nitro-1h-indazole

HRID 593110
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HRID 593110 반응식
Cl[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[C:11](=O)[CH3:12].Cl.[CH3:15][N:16](C)[NH2:17]>C(O)C>[CH3:15][N:16]1[C:2]2[C:3](=[CH:4][C:5]([N+:8]([O-:10])=[O:9])=[CH:6][CH:7]=2)[C:11]([CH3:12])=[N:17]1
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참가 물질

4

반응물 2

HCID 739511,1-Dimethylhydrazine monohydrochlorideHCID 899961-(2-Chloro-5-nitrophenyl)ethan-1-one

생성물 1

HCID 2909341,3-Dimethyl-5-nitro-1h-indazole수율 627.7%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 1-(2-chloro-5-nitrophenyl)ethanone (500 mg, 2.5 mmol) in anhydrous ethanol (15 mL) was added 1,1-dimethylhydrazine hydrochloride (3.38 g, 35.0 mmol) under nitrogen protection. The mixture was heated at reflux for 10 h and evaporated under reduced pressure to afford crude 307a (3.0 g), which was used in the next step without further purification. MS-ESI: [M+H]+ 192.2

후처리

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 10 h
  3. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-d6d238392bb4429aa51a53ffd6491e77
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09238655B2

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