Water → 3-Amino-1-(3-bromophenyl)butan-2-ol
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[Br:1][C:2]1[CH:3]=[C:4]([CH2:8][CH:9]([OH:15])[CH:10]([N+:12]([O-])=O)[CH3:11])[CH:5]=[CH:6][CH:7]=1.O>CCO.[Fe]>[NH2:12][CH:10]([CH3:11])[CH:9]([OH:15])[CH2:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([Br:1])[CH:3]=1참가 물질
5
실험 절차
To a solution of 1-(3-bromophenyl)-3-nitrobutan-2-ol (1.0 g, 3.6 mmol) in EtOH (20 mL)/H2O (1 mL), iron powder (2.0 g, 36 mmol) was added in one portion. The suspension was refluxed overnight, cooled to RT, and filtered. The filtrate was evaporated, diluted with H2O (30 mL), and extracted with EtOAc (50 mL×3). The organic layers were combined, dried over Na2SO4, filtered and concentrated. The residue was purified by silica gel column chromatography (Petroleum ether:EtOAc=3:1) to afford 3-amino-1-(3-bromophenyl)butan-2-ol (600 mg, 68%). MS (ES+) C10H14BrNO requires: 243, 245 found: 244, 246[M+2+H]+(1:1).
후처리
- temperatureThe suspension was refluxed overnight
- filtrationfiltered
- customThe filtrate was evaporated
- additiondiluted with H2O (30 mL)
- extractionextracted with EtOAc (50 mL×3)
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customThe residue was purified by silica gel column chromatography (Petroleum ether:EtOAc=3:1)
출처 및 근거
- ORD 기록
- ord-0340d367f73349b7959fb17d4d28e168
- 출처 데이터셋
- uspto-grants-2015_08
- 특허 번호
- US09115120B2
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