Hydrazine hydrate (1:1) → trans 5-(-2-methylcyclopropyl)-1H-pyrazol-3-amine

HRID 1484959노트

반응식

HRID 1484959 반응식
[CH3:1][CH:2]1[CH2:4][CH:3]1[C:5](=O)[CH2:6][C:7]#[N:8].O.[NH2:11][NH2:12]>C(O)C>[CH3:1][C@@H:2]1[CH2:4][C@H:3]1[C:5]1[NH:12][N:11]=[C:7]([NH2:8])[CH:6]=1

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 431156733-(2-Methylcyclopropyl)-3-oxopropanenitrile

생성물 1

HCID 51675220trans 5-(-2-methylcyclopropyl)-1H-pyrazol-3-amine수율 79%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

The crude 3-(2-methylcyclopropyl)-3-oxopropanenitrile was dissolved in ethanol (50 mL) and hydrazine hydrate (0.83 mL, 17 mmol) was added. The solution was maintained at reflux for 10 hours and then the solvent evaporated under vacuum. The residue was redissolved in methylene chloride and washed several times with brine. The organic layer was dried over anhydrous sodium sulfate and the solvent evaporated to give compound trans 5-(−2-methylcyclopropyl)-1H-pyrazol-3-amine (1 g, 79%, three step).

후처리

  1. temperatureThe solution was maintained
  2. temperatureat reflux for 10 hours
  3. customthe solvent evaporated under vacuum
  4. dissolutionThe residue was redissolved in methylene chloride
  5. washwashed several times with brine
  6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  7. customthe solvent evaporated

출처 및 근거

ORD 기록
ord-f054e4e6d4c74c10b448aec12f03042d
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09422271B2

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