반응식
[H-].[H-].[H-].[H-].[Li+].[Al+3].CN(OC)[C:9]([C@@H:11]([NH:14][C:15](=[O:21])[O:16][C:17]([CH3:20])([CH3:19])[CH3:18])[CH2:12][CH3:13])=[O:10]>CCOCC>[CH:9]([C@@H:11]([NH:14][C:15](=[O:21])[O:16][C:17]([CH3:20])([CH3:19])[CH3:18])[CH2:12][CH3:13])=[O:10]참가 물질
4
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- 온도
- 0 °C
실험 절차
To a solution of LiAlH4 (0.453 g, 11.9 mmol) in Et2O (20 mL) at 0° C. was added dropwise a solution of 1,1-dimethylethyl ((1S)-1-{[methyl(methyloxy)amino]carbonyl}-propyl)carbamate (2.67 g, 10.8 mmol) in Et2O (15 mL). The reaction mixture was stirred for 30 min at 0° C. and quenched with EtOAc (6.5 mL) followed by 5% aq. potassium bisulfate (6.5 mL). The reaction mixture was washed with 1 M aq. HCl (3×10 mL), saturated aq. NaHCO3 (3×10 mL), and brine (10 mL). The organic layer was dried over Na2SO4, filtered, and concentrated in vacuo to afford the title compound as a clear, colorless oil.
후처리
- customquenched with EtOAc (6.5 mL)
- washThe reaction mixture was washed with 1 M aq. HCl (3×10 mL), saturated aq. NaHCO3 (3×10 mL), and brine (10 mL)
- dry with materialThe organic layer was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated in vacuo
출처 및 근거
- ORD 기록
- ord-5760667bccfa440ab1833c283b8e4596
- 출처 데이터셋
- uspto-grants-2014_09
- 특허 번호
- US08841463B2
연결된 노트
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