Pyridine → HCID 178430970、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:12])=[CH:4][C:3]=1[N+:14]([O-:16])=[O:15].S(N)([NH2:20])(=O)=O.N1C=CC=CC=1>O>[CH3:1][C:2]1[C:7]2[NH:8][CH:9]=[N:10][C:6]=2[C:5]([C:11]([NH2:20])=[O:12])=[CH:4][C:3]=1[N+:14]([O-:16])=[O:15]参加物
5
実験手順
A mixture of 7-Methyl-6-nitro-1H-benzimidazole-4-carboxylic Acid (23) (0.692 g, 3.12 mmol), sulfamide (0.600 g, 6.26 mmol), and pyridine (8 mL) is heated at reflux for about 16 hours. The resulting heterogeneous reaction mixture is cooled to ambient temperature, diluted with water (10 mL) and cooled to 0° C. for 1 hour. The solids that form are filtered, washed with water (10 mL) and methanol (10 mL), and dried to obtain 7-Methyl-6-nitro-1H-benzimidazole-4-carboxamide (25) as a cream colored solid (0.586 g, 85% yield).
後処理
- temperatureis heated
- temperatureat reflux for about 16 hours
- temperaturecooled to 0° C. for 1 hour
- filtrationThe solids that form are filtered
- washwashed with water (10 mL) and methanol (10 mL)
- customdried
出典と根拠
- ORDレコード
- ord-133e330d35fb4bce9aa6ed0269430265
- 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…