反应详情

温度

100 °C

2-Oxo-1,2-dihydroquinoxaline-6-carbonitrile was suspended in POCl3 (25 mL) and DMF (10 drops) was added. The mixture was heated at 100° C. for 2 h, cooled and concentrated under reduced pressure to leave a black residue. The residue was dissolved in CH2Cl2 (200 mL), washed with satd aq NaHCO3 (25 mL) and brine (25 mL) and dried over Na2SO4. Removal of the solvent left an off white solid (4.50 g). A 0.50-g portion was purified by chromatography on a 40-g silica gel cartridge eluted with a 0-50% EtOAc in hexanes gradient to afford 2-chloroquinoxaline-6-carbonitrile (118 mg). LC-MS Method 1 tR=1.42 min, m/z=190.

1. temperaturecooled
2. concentrationconcentrated under reduced pressure
3. customto leave a black residue
4. washwashed with satd aq NaHCO3 (25 mL) and brine (25 mL)
5. dry with materialdried over Na2SO4
6. customRemoval of the solvent
7. waitleft an off white solid (4.50 g)
8. customA 0.50-g portion was purified by chromatography on a 40-g silica gel cartridge
9. washeluted with a 0-50% EtOAc in hexanes gradient