反応式
[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]参加物
4
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-244e704eab064c4daa8d3aa73bb770ea
- 出典データセット
- uspto-grants-2013_03
- 特許番号
- US08389736B2
関連ノート
読み込み中…