Pentanenitrile, 4,4-dimethyl-3-oxo- → 4-(5-Amino-3-tert-butyl-1H-pyrazol-1-yl)benzonitrile

HRID 220222ノート

反応式

HRID 220222 の反応式
Cl.[NH:2]([C:4]1[CH:11]=[CH:10][C:7]([C:8]#[N:9])=[CH:6][CH:5]=1)[NH2:3].[CH3:12][C:13]([CH3:20])([CH3:19])[C:14](=O)[CH2:15][C:16]#[N:17]>CO>[NH2:17][C:16]1[N:2]([C:4]2[CH:11]=[CH:10][C:7]([C:8]#[N:9])=[CH:6][CH:5]=2)[N:3]=[C:14]([C:13]([CH3:20])([CH3:19])[CH3:12])[CH:15]=1

参加物

4

反応物 2

HCID 108871Pentanenitrile, 4,4-dimethyl-3-oxo-HCID 162129624-Cyanophenylhydrazine Hydrochloride

生成物 1

HCID 71470834-(5-Amino-3-tert-butyl-1H-pyrazol-1-yl)benzonitrile収率 82.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A flask was charged with 4-hydrazinylbenzonitrile hydrochloride (0.70 g, 3.8 mmol.), 4,4-dimethyl-3-oxopentanenitrile (0.48 g, 3.8 mmol) and MeOH and the reaction was heated at refluxed overnight. The reaction was cooled, and the solids which formed upon cooling were filtered off and discarded. Additional solids formed upon further standing (product) along with product material in solution. The solution containing, the solids was concentrated to yield 0.75 g of solid product (92%). MS M+1 (241).

後処理

  1. temperaturethe reaction was heated
  2. temperatureat refluxed overnight
  3. temperatureThe reaction was cooled
  4. customthe solids which formed
  5. temperatureupon cooling
  6. filtrationwere filtered off
  7. customAdditional solids formed upon further standing (product) along with product material in solution
  8. additionThe solution containing
  9. concentrationthe solids was concentrated

出典と根拠

ORDレコード
ord-47f23733431e4f64928cf6f1025ffbcb
出典データセット
uspto-grants-2012_06
特許番号
US08202899B2

反応ノート

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