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Hydrazine → 6-Nitro-1H-indazol-3-amine

HRID 1163370
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HRID 1163370 반응식
F[C:2]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[CH:7]=[CH:6][C:3]=1[C:4]#[N:5].[NH2:13][NH2:14]>C(O)(C)C>[NH2:5][C:4]1[C:3]2[C:2](=[CH:9][C:8]([N+:10]([O-:12])=[O:11])=[CH:7][CH:6]=2)[NH:14][N:13]=1
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참가 물질

4

반응물 2

HCID 9321HydrazineHCID 27590482-Fluoro-4-nitrobenzonitrile

생성물 1

HCID 534045076-Nitro-1H-indazol-3-amine

시약·촉매·용매 1

HCID 3776Isopropanol용매

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온도
80 °C

실험 절차

To a solution of 2-fluoro-4-nitrobenzonitrile (10 mmol) in isopropanol (30 mL) was added aqueous hydrazine (4 mL). The resulting solution was heated at 80° C. for 12 h. The reaction mixture was then concentrated, water (30 mL) was added, and the solution was extracted with ethyl acetate (2×25 mL). The combined organics were washed with water (30 mL) and brine (30 mL) and dried over anhydrous sodium sulfate. The volatiles were removed in vacuo yielding 3-amino-6-nitroindazole as an orange solid, which was utilized for further transformation without further purification.

후처리

  1. concentrationThe reaction mixture was then concentrated
  2. additionwater (30 mL) was added
  3. extractionthe solution was extracted with ethyl acetate (2×25 mL)
  4. washThe combined organics were washed with water (30 mL) and brine (30 mL)
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe volatiles were removed in vacuo

출처 및 근거

ORD 기록
ord-108f43d122d944afa490bc413464fec5
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07820821B2

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