Methanol → HCID 178497357、化合物
反応式
[Cl:1][CH2:2][C:3]1[NH:7][C:6]2[CH:8]=[CH:9][C:10]([C:12]([OH:14])=[O:13])=[CH:11][C:5]=2[N:4]=1.S(=O)(=O)(O)O.[CH3:20]O>>[Cl:1][CH2:2][C:3]1[NH:7][C:6]2[CH:8]=[CH:9][C:10]([C:12]([O:14][CH3:20])=[O:13])=[CH:11][C:5]=2[N:4]=1参加物
4
実験手順
To 2-(Chloromethyl)-1H-benzimidazole-5-carboxylic acid (4) (0.5 g; 2.4 mmole) suspended in anhydrous methanol (20 ml) was added dropwise Sulfuric acid (0.2 ml). The reaction mixture was maintained at reflux for 16 hours. The solvent was evaporated to give the crude oily product, which was purified by column chromatography (silica, 10% methanol: dichloromethane) to obtain 0.4 g (71% yield) of product 5.
後処理
- temperatureThe reaction mixture was maintained
- temperatureat reflux for 16 hours
- customThe solvent was evaporated
- customto give the crude oily product, which
- customwas purified by column chromatography (silica, 10% methanol: dichloromethane)
出典と根拠
- ORDレコード
- ord-868a4287ec894ad8a8a4bf6d592a44da
- 出典データセット
- uspto-grants-2006_04
- 特許番号
- US07030150B2
反応ノート
読み込み中…