反応式
[CH3:1][O:2][C:3](=[O:31])[CH:4]([CH2:24][C:25]1[CH:30]=[CH:29][N:28]=[CH:27][CH:26]=1)[CH:5]([C:7]1[N:11]([CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[Cl:19])[C:10]([CH2:20][CH2:21][CH2:22][CH3:23])=[N:9][CH:8]=1)[OH:6].[C:32](OC(=O)C)(=[O:34])[CH3:33].O>CN(C)C1C=CN=CC=1.ClCCl.C(=O)(O)[O-].[Na+]>[CH3:1][O:2][C:3](=[O:31])[CH:4]([CH2:24][C:25]1[CH:30]=[CH:29][N:28]=[CH:27][CH:26]=1)[CH:5]([O:6][C:32](=[O:34])[CH3:33])[C:7]1[N:11]([CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[Cl:19])[C:10]([CH2:20][CH2:21][CH2:22][CH3:23])=[N:9][CH:8]=1参加物
反応物 3
生成物 1
試薬・触媒・溶媒 3
実験手順
A solution of methyl-3-[2-n-butyl-1-(2-chlorophenyl)methyl-1H-imidazol-5-yl]-3-hydroxy-2-[(4-pyridyl)methyl]propanoate (3.32 g, 7.5 mmol) dichloromethane (50 mL), 4-dimethylaminopyridine (150 mg, 1.3 mmol) and acetic anhydride (7.1 mL, 75 mmol) was stirred at ambient temperature for 18 hours. Water (5 mL) was added, the mixture was stirred for 2 hours and then diluted with dichloromethane and 5% sodium bicarbonate solution. The organic phase was washed with 5% sodium bicarbonate solution and brine, dried and concentrated to give 4 g of the crude title compound. TLC on silica gel with 5% methanol methyl-acetate showed essentially one spot material with an Rf of 0.86. No starting material was detected. This material was not purified further.
後処理
- washThe organic phase was washed with 5% sodium bicarbonate solution and brine
- customdried
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-c3709c55688c4bc3830dbd69e21491c5
- 出典データセット
- uspto-grants-1993_01
- 特許番号
- US05177096
関連ノート
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