HCID 58011039、化合物 → 3-[5-Amino-3-(1,1-dimethylethyl)-1H-pyrazol-1-yl]benzonitrile

HRID 1696425ノート

反応式

HRID 1696425 の反応式
[NH2:1][C:2]1[N:6]([C:7]2[CH:8]=[C:9]([CH:13]=[CH:14][CH:15]=2)[C:10]([NH2:12])=O)[N:5]=[C:4]([C:16]([CH3:19])([CH3:18])[CH3:17])[CH:3]=1>O=S(Cl)Cl>[NH2:1][C:2]1[N:6]([C:7]2[CH:8]=[C:9]([CH:13]=[CH:14][CH:15]=2)[C:10]#[N:12])[N:5]=[C:4]([C:16]([CH3:19])([CH3:18])[CH3:17])[CH:3]=1

参加物

3

反応物 1

HCID 58011039HCID 58011039、化合物

生成物 1

HCID 435430033-[5-Amino-3-(1,1-dimethylethyl)-1H-pyrazol-1-yl]benzonitrile収率 73%

試薬・触媒・溶媒 1

HCID 24386Thionyl Chloride溶媒

実験手順

A solution of 3-(5-amino-3-t-butyl-1H-pyrazol-1-yl)benzamide (5.2 g, 20 mmol) in SOCl2 (50 mL) was heated at reflux for 6 h. After removal of the solvent, the residue was dissolved in EtOAc (100 mL). The organic layer was washed with saturated NaHCO3 and brine, dried (Na2SO4), filtered, and purified by column chromatography to afford 3-(5-amino-3-t-butyl-1H-pyrazol-1-yl)benzonitrile (3.5 g, 73% yield).

後処理

  1. temperatureat reflux for 6 h
  2. customAfter removal of the solvent
  3. dissolutionthe residue was dissolved in EtOAc (100 mL)
  4. washThe organic layer was washed with saturated NaHCO3 and brine
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. custompurified by column chromatography

出典と根拠

ORDレコード
ord-6d00e7b6afe447f98b3eb79682f1b644
出典データセット
uspto-grants-2012_04
特許番号
US08163756B2

反応ノート

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