Methanol → 3-[4-Methoxy-3-[N-(4-trifluoromethylbenzyl)]carbamoylphenyl]-2-(methylsulfonyl)propionic acid
반응식
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]=1참가 물질
반응 조건
- 온도
- 50 °C
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-0c630759926242ef94b950911f87a8af
- 출처 데이터셋
- uspto-grants-2004_03
- 특허 번호
- US06706763B1
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