Phosphorus oxychloride → 8-Bromo-2-chloroquinoxaline
反応式
[Br:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:11]=1[NH:10][C:9](=O)[CH:8]=[N:7]2.O=P(Cl)(Cl)[Cl:15]>>[Br:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:11]=1[N:10]=[C:9]([Cl:15])[CH:8]=[N:7]2参加物
3
反応条件
- 温度
- 50 °C
実験手順
A mixture of 2.0 g (ca. 7.64 mmol) 8-Bromo-1H-quinoxalin-2-one and 36 ml of POCl3 is heated to 50° C. for 16 h. After cooling, the excess of POCl3 is evaporated, water is then added and extracted 3× with CH2Cl2. The combined organic layers are successively washed with water, NaHCO3, saturated brine, dried over Na2SO4, filtered and the filtrate is concentrated in vacuo. The residue is purified by chromatography (silicagel, hexane:CH2Cl2=7:3=>1:1) to afford the title compound as a pale orange solid, MS: 243 (M)+
後処理
- temperatureAfter cooling
- customthe excess of POCl3 is evaporated
- additionwater is then added
- extractionextracted 3× with CH2Cl2
- washThe combined organic layers are successively washed with water, NaHCO3, saturated brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationthe filtrate is concentrated in vacuo
- customThe residue is purified by chromatography (silicagel, hexane:CH2Cl2=7:3=>1:1)
出典と根拠
- ORDレコード
- ord-d17185f5bce94effaf1c9d3a0087e6ea
- 出典データセット
- uspto-grants-2012_06
- 特許番号
- US08193189B2
反応ノート
読み込み中…