반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]([CH3:19])([CH3:18])[C:16]#[N:17])=[CH:11][CH:10]=1.[OH-].[Na+].O>C(OCC)C>[CH3:7][O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]([CH3:19])([CH3:18])[CH2:16][NH2:17])=[CH:11][CH:10]=1참가 물질
반응 조건
- 온도
- 5 °C
실험 절차
A reaction vessel was charged with lithiumaluminium hydride (0.433 g, 11.41 mmol) and dry diethyl ether (20 mL). After cooling to 5° C. a solution of 2-(4-methoxyphenyl)-2-methylpropanenitrile (2.00 g, 11.41 mmol) in dry diethylether (10 mL) was added dropwise. The reaction mixture was stirred at 5° C. for 2 h. The reaction mixture was then cooled in an ice bath and 2N aqueous sodium hydroxide solution (0.8 mL) and water (1.5 mL) were added. After stirring for 20 min additional water (40 mL) was added and the reaction mixture was extracted with ethyl acetate (2×30 mL). The combined extracts were dried (MgSO4) and the solvent was evaporated in vacuo. The crude product (1.94 g, 10.82 mmol) was used without further purification for the next step.
후처리
- additionwas added dropwise
- temperatureThe reaction mixture was then cooled in an ice bath
- additionwas added
- extractionthe reaction mixture was extracted with ethyl acetate (2×30 mL)
- dry with materialThe combined extracts were dried (MgSO4)
- customthe solvent was evaporated in vacuo
출처 및 근거
- ORD 기록
- ord-136d45100f5e456f8a709651efd03beb
- 출처 데이터셋
- uspto-grants-2014_02
- 특허 번호
- US08653100B2
연결된 노트
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