3-[(3-Nitro-1H-pyrazol-1-yl)methyl]benzonitrile → 3-((3-Amino-1h-pyrazol-1-yl)methyl)benzonitrile

HRID 18958노트

반응식

HRID 18958 반응식
[N+:1]([C:4]1[CH:8]=[CH:7][N:6]([CH2:9][C:10]2[CH:11]=[C:12]([CH:15]=[CH:16][CH:17]=2)[C:13]#[N:14])[N:5]=1)([O-])=O>C(O)C.[Pd]>[NH2:1][C:4]1[CH:8]=[CH:7][N:6]([CH2:9][C:10]2[CH:11]=[C:12]([CH:15]=[CH:16][CH:17]=2)[C:13]#[N:14])[N:5]=1

참가 물질

4

반응물 1

HCID 617213403-[(3-Nitro-1H-pyrazol-1-yl)methyl]benzonitrile

생성물 1

HCID 607831823-((3-Amino-1h-pyrazol-1-yl)methyl)benzonitrile수율 64.3%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

A solution of 3-(3-nitro-pyrazol-1-ylmethyl)-benzonitrile (507 mg, 2.22 mmol) in ethanol (25 mL) was hydrogenated in a Parr hydrogenator using 10% palladium on carbon (53 mg, 0.05 mmol) for 4 h at 50 psi at room temperature. The product was isolated, after filtration through a Celite plug, and purification by ISCO flash chromatography (Teledyne Isco RediSep Flash Column 4 g; 0% to 10% methanol/dichloromethane) to afford 3-(3-amino-pyrazol-1-ylmethyl)-benzonitrile, (283 mg, 64%) as light orange solid.

후처리

  1. customfor 4 h
  2. customat room temperature
  3. customThe product was isolated
  4. filtrationafter filtration
  5. customthrough a Celite plug, and purification by ISCO flash chromatography (Teledyne Isco RediSep Flash Column 4 g; 0% to 10% methanol/dichloromethane)

출처 및 근거

ORD 기록
ord-983251181e004aef93b38d02e17cf7f7
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07741327B2

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