Formic Acid → HCID 178425875、化合物
反応式
[NH2:1][C:2]1[C:3]([N+:12]([O-])=O)=[C:4]([CH:8]=[CH:9][C:10]=1[CH3:11])[C:5]([OH:7])=[O:6].[CH:15](O)=O>[Pd]>[CH3:11][C:10]1[C:2]2[NH:1][CH:15]=[N:12][C:3]=2[C:4]([C:5]([OH:7])=[O:6])=[CH:8][CH:9]=1参加物
4
実験手順
A mixture of 3-amino-4-methyl-2-nitrobenzoic acid (16) (6.883 g, 35.10 mmol), 10% Pd/C [0.3 g, 10% dry Pd/C] and 75% aqueous formic acid (60 mL) is heated to reflux for about 15 hours. The reaction mixture is then cooled to ambient temperature and filtered through a pad of Celite, and the resulting filtrate concentrated in vacuo to a beige solid. The solids are triturated in hot methanol (50 mL), cooled slowly to ambient temperature, and filtered to give 7-Methyl-1H-benzimidazole-4-carboxylic Acid (22), as beige solid (5.26 g, 85% Yield).
後処理
- temperatureis heated
- temperatureto reflux for about 15 hours
- filtrationfiltered through a pad of Celite
- concentrationthe resulting filtrate concentrated in vacuo to a beige solid
- customThe solids are triturated in hot methanol (50 mL)
- temperaturecooled slowly to ambient temperature
- filtrationfiltered
出典と根拠
- ORDレコード
- ord-e018647eec924f3fa6e9013f2822ea05
- 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…