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

HRID 968788노트

반응식

HRID 968788 반응식
[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]

참가 물질

4

반응물 1

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

생성물 1

HCID 178430523HCID 178430523, 화합물수율 102.2%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

반응 조건

온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-80b7e7436e144163af9fee8ac0584584
출처 데이터셋
uspto-grants-2007_12
특허 번호
US07304084B2

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