Hydrochloric Acid → 1H-Imidazole-2-propanol, 5-((3,5-dichlorophenyl)thio)-1-(2-hydroxyethyl)-4-(1-methylethyl)-
反応式
Cl.C([O:9][CH2:10][CH2:11][CH2:12][C:13]1[N:14]([CH2:30][CH2:31][OH:32])[C:15]([S:21][C:22]2[CH:27]=[C:26]([Cl:28])[CH:25]=[C:24]([Cl:29])[CH:23]=2)=[C:16]([CH:18]([CH3:20])[CH3:19])[N:17]=1)C1C=CC=CC=1.C(=O)([O-])O.[Na+]>>[Cl:29][C:24]1[CH:23]=[C:22]([S:21][C:15]2[N:14]([CH2:30][CH2:31][OH:32])[C:13]([CH2:12][CH2:11][CH2:10][OH:9])=[N:17][C:16]=2[CH:18]([CH3:20])[CH3:19])[CH:27]=[C:26]([Cl:28])[CH:25]=1参加物
4
反応条件
- 温度
- 110 °C
実験手順
To 14 ml of concentrated hydrochloric acid, 1.4 g (2.9 mmol)of the alcohol (136e)was added and the mixture was heated at 110° C. for 7 hours. After cooling, the mixture was neutralized with sodium hydrogen carbonate and extracted with ethyl acetate. The extract was washed with water, dried over sodium sulfate, filtered, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (5% methanol-ethyl acetate)to provide 300 mg (yield 26%)of 3-(5-(3,5-dichlorophenylthio)-1-(2-hydroxyethyl)-4-isopropyl-1H-imidazol-2-yl)-propan-1-ol (137d)as oil.