Lithium hydroxide, monohydrate → 5-Ethyl-3-phenyl-1,2-oxazole-4-carboxylic acid
반응식
C[O:2][C:3]([C:5]1[C:6]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[N:7][O:8][C:9]=1[CH2:10][CH3:11])=[O:4].O[Li].O>C1COCC1.O>[CH2:10]([C:9]1[O:8][N:7]=[C:6]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[C:5]=1[C:3]([OH:4])=[O:2])[CH3:11]참가 물질
5
실험 절차
To a solution of 5-ethyl-3-phenyl-isoxazole-4-carboxylic acid methyl ester (12.0 g, 51 mmol) in THF (50 mL), was added a solution of LiOH.H2O (10.8 g, 255 mmol) in water (25 mL) in one portion. The reaction mixture was then heated under reflux for 12 h. After cooling to room temperature and concentration, the remaining mixture was extracted with ethyl acetate and dried over sodium sulphate. Evaporation afforded the title compound (8.01 g, 72%) as yellow solid. MS: m/e=218.1 [M+H]+.
후처리
- temperatureThe reaction mixture was then heated
- temperatureunder reflux for 12 h
- concentrationconcentration
- extractionthe remaining mixture was extracted with ethyl acetate
- dry with materialdried over sodium sulphate
- customEvaporation
출처 및 근거
- ORD 기록
- ord-4877205193f3444d989c7ce319d59308
- 출처 데이터셋
- uspto-grants-2008_08
- 특허 번호
- US07414061B2
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