反応式
Cl[CH2:2][C:3]1[CH:19]=[CH:18][C:6]([C:7]([NH:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[O:16][CH3:17])=[O:8])=[CH:5][CH:4]=1.[OH-].[Na+].CO.C1C[O:27][CH2:26]C1>>[CH3:26][O:27][CH2:2][C:3]1[CH:19]=[CH:18][C:6]([C:7]([NH:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[O:16][CH3:17])=[O:8])=[CH:5][CH:4]=1参加物
4
実験手順
4-Chloromethyl-N-(2-methoxyphenyl)benzamide (138 mg, 0.50 mmol) was dissolved in a methanol-THF (1:1) mixture solution (6 ml) to which was subsequently added 10% sodium hydroxide aqueous solution (3 ml) at room temperature. After 14 hours of stirring at the same temperature, the reaction solution was subjected to 3 hours of ultrasonic treatment. After removing the organic solvent by evaporation, the resulting residue was extracted with methylene chloride and dried on anhydrous magnesium sulfate. After removing the solvent by evaporation, the resulting colorless oily material was purified by silica gel column chromatography (ether:hexane=1:2) to obtain 126 mg (92.9%) of the title compound in the form of colorless oil.
後処理
- customat room temperature
- waitthe reaction solution was subjected to 3 hours of ultrasonic treatment
- customAfter removing the organic solvent
- customby evaporation
- extractionthe resulting residue was extracted with methylene chloride
- dry with materialdried on anhydrous magnesium sulfate
- customAfter removing the solvent
- customby evaporation
- customthe resulting colorless oily material was purified by silica gel column chromatography (ether:hexane=1:2)
出典と根拠
- ORDレコード
- ord-ad335823cf4c4c7daba8d6b3227c7ced
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05728835
関連ノート
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