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

HRID 1484959ノート

反応式

HRID 1484959 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-f054e4e6d4c74c10b448aec12f03042d
出典データセット
uspto-grants-2016_08
特許番号
US09422271B2

反応ノート

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