Sodium Carbonate → 3-bromo-1-ethyl-quinoxalin-2(1H)-one
反応式
[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[NH:6][C:5](=O)[C:4]1=[O:14])[CH3:2].P(Br)(Br)([Br:17])=O.C(=O)([O-])[O-].[Na+].[Na+]>ClC(Cl)C>[Br:17][C:5]1[C:4](=[O:14])[N:3]([CH2:1][CH3:2])[C:12]2[C:7]([N:6]=1)=[CH:8][CH:9]=[CH:10][CH:11]=2参加物
5
実験手順
To 2 g (10.5 mM) of 1-ethyl-1,4-dihydroquinoxaline-2,3-dione in 20 ml of dichloroethane were added dropwise 3.16 g (11.0 mM) of POBr3. The reaction mixture was refluxed under stirring for 2 h and then treated with ice cold and an aqueous sodium carbonate solution. The mixture was filtered and the filtrate was extracted with dichloromethane, dried over anhydrous sodium sulfate and concentrated to give 1,4 g of 3-bromo-1-ethyl-quinoxalin-2(1H)-one as a yellow solid. Yield: 53%.
後処理
- temperatureThe reaction mixture was refluxed
- additiontreated with ice cold
- filtrationThe mixture was filtered
- extractionthe filtrate was extracted with dichloromethane
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-7da4a326928d43f3991e49751fbcc300
- 出典データセット
- uspto-grants-2013_04
- 特許番号
- US08415352B2
反応ノート
読み込み中…