Hydrazine → HCID 178507285, 화합물

HRID 1943905노트

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HRID 1943905 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7](=O)[CH2:8][C:9]#[N:10].[NH2:12][NH2:13]>C(O)C>[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7]1[CH:8]=[C:9]([NH2:10])[NH:13][N:12]=1

참가 물질

4

반응물 2

HCID 9321HydrazineHCID 115718233-Oxo-3-(pyridin-2-yl)propanenitrile

생성물 1

HCID 178507285HCID 178507285, 화합물수율 91%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

3-(2-Pyridyl)-3-oxopropanenitrile (3.0 g, 0.37 mol) was dissolved in ethanol (22 mL) and treated with hydrazine (1.9 mL, 0.062 mol) at reflux for 24 hours. The reaction mixture was concentrated, diluted with brine and extracted into ethyl acetate (2×50 mL). The combined organic layers were dried (MgSO4), concentrated and purified by silica gel chromatography eluting with 2-20% methanol in methylene chloride to afford 3-(pyridin-2-yl)-1H-pyrazol-5-amine (3.0 g, 91% yield).

후처리

  1. temperatureat reflux for 24 hours
  2. concentrationThe reaction mixture was concentrated
  3. additiondiluted with brine
  4. extractionextracted into ethyl acetate (2×50 mL)
  5. dry with materialThe combined organic layers were dried (MgSO4)
  6. concentrationconcentrated
  7. custompurified by silica gel chromatography
  8. washeluting with 2-20% methanol in methylene chloride

출처 및 근거

ORD 기록
ord-a1636b72dbbb4e759fb21ee6267195f9
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08394795B2

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