Hydrochloric Acid → Ethyl 2-amino-2-(4-bromophenyl)propanoate
반응식
[NH2:1][C:2]([C:7]1[CH:12]=[CH:11][C:10]([Br:13])=[CH:9][CH:8]=1)([CH3:6])[C:3]([OH:5])=[O:4].Cl.[CH2:15](O)[CH3:16]>>[CH2:15]([O:4][C:3](=[O:5])[C:2]([NH2:1])([C:7]1[CH:8]=[CH:9][C:10]([Br:13])=[CH:11][CH:12]=1)[CH3:6])[CH3:16]참가 물질
4
실험 절차
To a solution of 2-amino-2-(4-bromo-phenyl)-propionic acid (1.0 g, 4.1 mmol) in ethanol (20 mL) was bubbled through HCl gas for five minutes. The mixture was stirred at ambient for 24 hours, then refluxed for 18 hours. The volatile component was removed in vacuo, and the residue was dissolved in ethyl acetate (150 mL), washed with NaHCO3 solution, water and brine, dried over MgSO4, filtered and concentrated in vacuo. The obtained residue was purified by flash chromatography to provide the desired product (800 mg, 72%). m/z 271.7, 273.7 (M+H)+.
후처리
- temperaturerefluxed for 18 hours
- customThe volatile component was removed in vacuo
- dissolutionthe residue was dissolved in ethyl acetate (150 mL)
- washwashed with NaHCO3 solution, water and brine
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe obtained residue was purified by flash chromatography
출처 및 근거
- ORD 기록
- ord-229ad93c4cd04596bc78cc2c125ccf81
- 출처 데이터셋
- uspto-grants-2014_03
- 특허 번호
- US08669234B2
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