Methanol → 3-[4-Methoxy-3-[N-(4-trifluoromethylbenzyl)]carbamoylphenyl]-2-(methylsulfonyl)propionic acid
反応式
CO.[CH3:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][CH:12]([S:17]([CH3:20])(=[O:19])=[O:18])[C:13]([O:15]C)=[O:14])=[CH:7][C:6]=1[C:21](=[O:34])[NH:22][CH2:23][C:24]1[CH:29]=[CH:28][C:27]([C:30]([F:33])([F:32])[F:31])=[CH:26][CH:25]=1.[OH-].[Na+]>O>[CH3:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][CH:12]([S:17]([CH3:20])(=[O:18])=[O:19])[C:13]([OH:15])=[O:14])=[CH:7][C:6]=1[C:21](=[O:34])[NH:22][CH2:23][C:24]1[CH:25]=[CH:26][C:27]([C:30]([F:31])([F:33])[F:32])=[CH:28][CH:29]=1参加物
反応条件
- 温度
- 50 °C
実験手順
Into 6 ml of methanol were dissolved 300 mg of methyl 3-[4-methoxy-3-[N-(4-trifluoromethylbenzyl)]carbamoylphenyl]-2-(methylsulfonyl)propionate, 0.7 ml of 1 mol/l aqueous solution of sodium hydroxide were added, and the mixture was stirred for 1 hour at 50° C. The reaction mixture was poured into water and washed with diethyl ether. The aqueous layer was adjusted to pH value of 1 to 2 with 2 mol/l aqueous solution of hydrochloric acid, which was extracted with methylene chloride. The organic layer was washed with water and saturated brine in sequence and dried over anhydrous sodium sulfate. Solvent was distilled off under reduced pressure, and the crystals obtained were recrystallized from diethyl ether-ethyl acetate to obtain 218 mg of aimed product as colorless crystals.
後処理
- additionwere added
- washwashed with diethyl ether
- extractionwas extracted with methylene chloride
- washThe organic layer was washed with water and saturated brine in sequence
- dry with materialdried over anhydrous sodium sulfate
- distillationSolvent was distilled off under reduced pressure
- customthe crystals obtained
- customwere recrystallized from diethyl ether-ethyl acetate
出典と根拠
- ORDレコード
- ord-0c630759926242ef94b950911f87a8af
- 出典データセット
- uspto-grants-2004_03
- 特許番号
- US06706763B1
反応ノート
読み込み中…