Phosphorus oxychloride → HCID 178430969、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](O)=O)=[CH:4][C:3]=1[N+:14]([O-:16])=[O:15].O=P(Cl)(Cl)Cl.S(N)([NH2:25])(=O)=O>S1(CCCC1)(=O)=O>[CH3:1][C:2]1[C:7]2[NH:8][CH:9]=[N:10][C:6]=2[C:5]([C:11]#[N:25])=[CH:4][C:3]=1[N+:14]([O-:16])=[O:15]参加物
5
反応条件
- 温度
- 120 °C
実験手順
A mixture of 7-Methyl-6-nitro-1H-benzimidazole-4-carboxylic Acid (23) (16.99 g, 76.90 mmol), POCl3 (15.76 mL, 169 mmol), and sulfamide (14.767 g, 154 mmol) in sulfolane (77 mL) is heated to about 120° C. for about 3 hours. The reaction mixture is cooled to ambient temperature and added to ice water (1 L). The resultant mixture is cooled to about 0° C. filtered to provide 7-Methyl-6-nitro-1H-benzimidazole-4-carbonitrile (24), as an off white solid (12.54 g, 80% Yield).
後処理
- temperatureThe reaction mixture is cooled to ambient temperature
- filtrationfiltered
出典と根拠
- ORDレコード
- ord-04deb647738c4d0eaf145939f96f16da
- 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…