Cyclopentylhydrazine hydrochloride → 1-cyclopentyl-3-ethyl-4-cyano-5-amino-1H-pyrazole

HRID 487246

反応式

HRID 487246 の反応式
Cl.[CH:2]1([NH:7][NH2:8])[CH2:6][CH2:5][CH2:4][CH2:3]1.C[O-].[Na+].C(O[C:15](=[C:18]([C:21]#[N:22])[C:19]#[N:20])[CH2:16][CH3:17])C>C(O)C>[CH:2]1([N:7]2[C:21]([NH2:22])=[C:18]([C:19]#[N:20])[C:15]([CH2:16][CH3:17])=[N:8]2)[CH2:6][CH2:5][CH2:4][CH2:3]1

参加物

5

反応物 3

HCID 212349Cyclopentylhydrazine hydrochlorideHCID 2314702-(1-Ethoxypropylidene)malononitrileHCID 10942334Sodium Methoxide

生成物 1

HCID 158712691-cyclopentyl-3-ethyl-4-cyano-5-amino-1H-pyrazole収率 70%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Cyclopentylhydrazine hydrochloride (20.9 g, 0.1 moles), 97% sodium methoxide (5.6 g, 0.1 moles) and ethanol (100 ml) were combined and stirred at room temperature under argon for 2.5 hours. (1-Ethoxypropylidene)malononitrile was added to the reaction mixture and the mixture was refluxed for 21 hours. The reaction mixture was cooled and the solvent was removed in vacuo. The residue was treated with water (150 ml) and the obtained precipitate was collected by filtration, washed with water and dried in a vacuum oven for 24 hours to afford 14.2 g (70%) of 1-cyclopentyl-3-ethyl-5-amino-1H-pyrazole-4-carbonitrile as a brown powder, m.p. 171°-173° C.

後処理

  1. temperaturethe mixture was refluxed for 21 hours
  2. temperatureThe reaction mixture was cooled
  3. customthe solvent was removed in vacuo
  4. additionThe residue was treated with water (150 ml)
  5. filtrationthe obtained precipitate was collected by filtration
  6. washwashed with water
  7. customdried in a vacuum oven for 24 hours

出典と根拠

ORDレコード
ord-91d4259f2de04cbc9ef990ea40a3c8a7
出典データセット
uspto-grants-1994_03
特許番号
US05294612

関連ノート

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