Hydrochloride methanol → 1-(3-Amino-3-methyl-butyl)-1,3-dihydro-benzimidazol-2-one
反応式
[CH3:1][C:2]([NH:16]C=O)([CH3:15])[CH2:3][CH2:4][N:5]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[NH:7][C:6]1=[O:14].Cl.CO>>[NH2:16][C:2]([CH3:15])([CH3:1])[CH2:3][CH2:4][N:5]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[NH:7][C:6]1=[O:14]参加物
3
実験手順
A mixture of N-[1,1-dimethyl-3-(2-oxo-2,3-dihydro-1H-benzimidazol-1-yl)propyl]formamide (1.1 g) and hydrogen chloride-methanol (80-90% methanol, 18 mL) was stirred at rt for 50 h. The mixture was concentrated in vacuo and the residue was basified by aq. potassium carbonate and the mixture was extracted with dichloromethane. The combined organic layers were dried over sodium sulfate and concentrated to give 0.81 g (3.7 mmol, 73% for 3 steps) of the title compound.
後処理
- concentrationThe mixture was concentrated in vacuo
- extractionthe mixture was extracted with dichloromethane
- dry with materialThe combined organic layers were dried over sodium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-c1ca561ee14c4682a0fb1bc14272255a
- 出典データセット
- uspto-grants-2012_03
- 特許番号
- US08138177B2
反応ノート
読み込み中…