反応式
[OH-].[Li+].[C:3]([O:7][C:8]([NH:10][CH2:11][CH2:12][CH2:13][N:14]1[C:18]2[CH:19]=[C:20]([C:23]([O:25]C)=[O:24])[CH:21]=[CH:22][C:17]=2[N:16]=[C:15]1[NH:27][C:28]1[CH:33]=[C:32]([O:34][CH3:35])[C:31]([O:36][CH3:37])=[C:30]([O:38][CH3:39])[CH:29]=1)=[O:9])([CH3:6])([CH3:5])[CH3:4]>O1CCCC1.O>[C:3]([O:7][C:8]([NH:10][CH2:11][CH2:12][CH2:13][N:14]1[C:18]2[CH:19]=[C:20]([C:23]([OH:25])=[O:24])[CH:21]=[CH:22][C:17]=2[N:16]=[C:15]1[NH:27][C:28]1[CH:29]=[C:30]([O:38][CH3:39])[C:31]([O:36][CH3:37])=[C:32]([O:34][CH3:35])[CH:33]=1)=[O:9])([CH3:5])([CH3:4])[CH3:6]参加物
5
反応物 2
生成物 1
試薬・触媒・溶媒 2
実験手順
Lithium hydroxide (2.18 g, 6 eq) is added to a solution of methyl 1-{3-[(tert-butoxycarbonyl)amino]propyl}-2-[(3,4,5-trimethoxyphenyl)amino]-1H-benzimidazole-6-carboxylate (4.4 g, 1 eq) in a mixture of tetrahydrofuran (40 ml) and water (30 ml). The mixture is heated under reflux for 18 hours then cooled down to ambient temperature and concentrated under reduced pressure at 40° C. Dichloromethane (150 ml) and water (100 ml) are added to the residue. The mixture is acidified by the addition of acetic acid to pH 5. After decantation and extractions, the combined organic phases are dried over sodium sulphate and concentrated under reduced pressure. The solid obtained is washed with ethyl ether (3.95 g; 93%).
後処理
- temperatureThe mixture is heated
- temperatureunder reflux for 18 hours
- concentrationconcentrated under reduced pressure at 40° C
- additionDichloromethane (150 ml) and water (100 ml) are added to the residue
- additionThe mixture is acidified by the addition of acetic acid to pH 5
- extractionAfter decantation and extractions
- dry with materialthe combined organic phases are dried over sodium sulphate
- concentrationconcentrated under reduced pressure
- customThe solid obtained
- washis washed with ethyl ether (3.95 g; 93%)
出典と根拠
- ORDレコード
- ord-f0068efb9ed942a5b8e5833afdaf3f83
- 出典データセット
- uspto-grants-2009_03
- 特許番号
- US07501525B2
関連ノート
読み込み中…