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Hydrazine hydrate (1:1) → 3,5-Diamino-4-(4-ethylphenylmethyl)pyrazole

HRID 1625851
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인쇄 미리보기

반응식

HRID 1625851 반응식
[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH:10]([C:13]#[N:14])[C:11]#[N:12])=[CH:5][CH:4]=1)[CH3:2].O.[NH2:16][NH2:17]>C(O)C>[NH2:12][C:11]1[C:10]([CH2:9][C:6]2[CH:5]=[CH:4][C:3]([CH2:1][CH3:2])=[CH:8][CH:7]=2)=[C:13]([NH2:14])[NH:17][N:16]=1
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)2회HCID 821115992-(4-Ethylphenylmethyl)malononitrile

생성물 1

HCID 666081683,5-Diamino-4-(4-ethylphenylmethyl)pyrazole

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of the above 2-(4-ethylphenylmethyl)malononitrile (1.30 g) and hydrazine hydrate (0.86 ml) in ethanol (35 ml) was heated under reflux for 4 hours. Hydrazine hydrate (0.43 ml) was further added thereto and the mixture was further heated under reflux for 4 hours. The reaction mixture was cooled to room temperature and the solvent was evaporated under reduced pressure. The residue was crystallized from ethyl acetate-diethyl ether to give 3,5-diamino-4-(4-ethylphenylmethyl)pyrazole (2.63 g) as pale pink powder. APCI-Mass m/Z 217 (M+H).

후처리

  1. temperatureunder reflux for 4 hours
  2. temperaturethe mixture was further heated
  3. temperatureunder reflux for 4 hours
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was crystallized from ethyl acetate-diethyl ether

출처 및 근거

ORD 기록
ord-03e4d7fb0cf249c1b50aa3aeae44957f
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08785403B2

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