N'-(6-Cyano-3-methyl-2,4-dinitro-phenyl)-N,N-dimethyl-methanimidamide → HCID 178430523、化合物

HRID 968788ノート

反応式

HRID 968788 の反応式
[C:1]([C:3]1[C:8]([N:9]=[CH:10]N(C)C)=[C:7]([N+:14]([O-])=O)[C:6]([CH3:17])=[C:5]([N+:18]([O-])=O)[CH:4]=1)#[N:2]>[Pd].CO>[NH2:18][C:5]1[CH:4]=[C:3]([C:1]#[N:2])[C:8]2[N:9]=[CH:10][NH:14][C:7]=2[C:6]=1[CH3:17]

参加物

4

反応物 1

HCID 59016305N'-(6-Cyano-3-methyl-2,4-dinitro-phenyl)-N,N-dimethyl-methanimidamide

生成物 1

HCID 178430523HCID 178430523、化合物収率 102.2%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

反応条件

温度
60 °C

実験手順

A mixture of N′-(6-cyano-3-methyl-2,4-dinitro-phenyl)-N,N-dimethyl-methanimidamide (8) (0.607 g, 2.42 mmol) and 10% palladium on carbon (0.23 g of 50% water wet) and methanol (60 mL) is agitated under hydrogen pressure (43 psi) for about 4.5 hours. The vessel is then flushed with nitrogen and the mixture is heated to 60° C. for about 2.5 hours. The mixture is allowed to cool to ambient temperature and is then filtered through a pad of Celite. The solvent is then evaporated in vacuo to provide 6-Amino-7-methyl-1H-benzimidazole-4-carbonitrile (10) (0.426 g, >100% crude Yield), as a brown solid.

後処理

  1. customThe vessel is then flushed with nitrogen
  2. temperatureto cool to ambient temperature
  3. filtrationis then filtered through a pad of Celite
  4. customThe solvent is then evaporated in vacuo

出典と根拠

ORDレコード
ord-80b7e7436e144163af9fee8ac0584584
出典データセット
uspto-grants-2007_12
特許番号
US07304084B2

反応ノート

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