반응식
[N+:1]([C:4]1[CH:5]=[C:6]([C:10](=[O:13])[CH2:11][CH3:12])[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2].[Br:14]Br>C(O)(=O)C>[Br:14][CH:11]([CH3:12])[C:10]([C:6]1[CH:7]=[CH:8][CH:9]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=1)=[O:13]참가 물질
4
실험 절차
To a stirred solution of 1-(3-nitrophenyl)propan-1-one (1.41 g, 7.90 mmol) in acetic acid (20 mL) was added bromine dropwise (1.27 g, 7.93 mmol) and the mixture was stirred at room temperature for 24 h. The mixture was poured into ice-cold water and the organic layer was extracted with DCM. The organic extract was washed with sat. aq. NaHCO3 and brine, dried over anhydrous MgSO4, and filtered. Evaporation of the solvent under reduced pressure afforded 11z as a white solid which was used in the next step without further purification (1.78 g, 87%). 1H NMR matches literature data.
후처리
- additionThe mixture was poured into ice-cold water
- extractionthe organic layer was extracted with DCM
- extractionThe organic extract
- washwas washed with sat. aq. NaHCO3 and brine
- dry with materialdried over anhydrous MgSO4
- filtrationfiltered
- customEvaporation of the solvent under reduced pressure
출처 및 근거
- ORD 기록
- ord-244e704eab064c4daa8d3aa73bb770ea
- 출처 데이터셋
- uspto-grants-2013_03
- 특허 번호
- US08389736B2
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