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

HRID 487246

반응식

HRID 487246 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-91d4259f2de04cbc9ef990ea40a3c8a7
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05294612

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