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Water → 4-iodo-1H-indazol-3-amine

HRID 560918
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인쇄 미리보기

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HRID 560918 반응식
F[C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([I:10])[C:3]=1[C:4]#[N:5].O.[NH2:12][NH2:13].O>C(O)CCC>[I:10][C:6]1[CH:7]=[CH:8][CH:9]=[C:2]2[C:3]=1[C:4]([NH2:5])=[N:12][NH:13]2
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참가 물질

5

반응물 3

HCID 962WaterHCID 24654Hydrazine hydrate (1:1)HCID 5227222-Fluoro-6-iodobenzonitrile

생성물 1

HCID 40577874-iodo-1H-indazol-3-amine

시약·촉매·용매 1

HCID 2631-Butanol용매

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온도
107.5 °C

실험 절차

A mixture of 2-fluoro-6-iodobenzonitrile (2 g, 8.1 mmol) and hydrazine hydrate (4 mL) in n-butanol (40 mL) was heated to 105-110° C. for 5 hours, cooled to room temperature, poured into water, and extracted twice with ethyl acetate. The combined extracts were washed with water and brine, dried (MgSO4), filtered, and concentrated to provide 1.88 g of the desired product. Rf=0.25 (5% methanol/dichloromethane).

후처리

  1. temperaturecooled to room temperature
  2. extractionextracted twice with ethyl acetate
  3. washThe combined extracts were washed with water and brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-c37be4e7cf5e49c49b9d81bd0459cb7b
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08063091B2

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