HCID 178418361、化合物 → HCID 178430523、化合物
反応式
[CH3:1][C:2]1[C:7]2[NH:8][CH:9]=[N:10][C:6]=2[C:5]([C:11]#[N:12])=[CH:4][C:3]=1[N+:13]([O-])=O.[H][H]>CN(C=O)C.[Pt]>[NH2:13][C:3]1[CH:4]=[C:5]([C:11]#[N:12])[C:6]2[N:10]=[CH:9][NH:8][C:7]=2[C:2]=1[CH3:1]参加物
5
実験手順
A mixture of 7-Methyl-6-nitro-1H-benzimidazole-4-carbonitrile (24) (1.010 g, 5.0 mmol) and Pt/C (5% Pt/C sulfided, 0.502 g, 50 wt %, C5002 Engelhard Industries) in DMF (75 mL) is hydrogenated at about 40 psi hydrogen pressure at about 50° C. over about 24 hours. The catalyst is removed from the reaction mixture by filtration through a Celite pad and the filtrate is concentrated in vacuo. The residue obtained is triturated in acetonitrile, and filtered to provide 6-Amino-7-methyl-1H-benzimidazole-4-carbonitrile (10), as a tan solid (0.768 g, 90% Yield).
後処理
- customThe catalyst is removed from the reaction mixture by filtration through a Celite pad
- concentrationthe filtrate is concentrated in vacuo
- customThe residue obtained
- customis triturated in acetonitrile
- filtrationfiltered
出典と根拠
- ORDレコード
- ord-58f400fa5f094b26ab26f318e775f936
- 出典データセット
- uspto-grants-2007_12
- 特許番号
- US07304084B2
反応ノート
読み込み中…