反应详情

At T=120° C., 30.0 g (60.0 mmol) of 2,7-dichloroquinoxaline are stirred in 400 ml of NH3/MeOH (w=22%) for 16 hours. The mixture is then evaporated to dryness under reduced pressure, and the residue is taken up in 250 ml of dichloromethane and 250 ml of water. After phase separation, the organic phase is then washed with 250 ml of water and dried over sodium sulphate, and the solvent is removed under membrane pump vacuum. The residue obtained is purified by column chromatography on silica gel (ethyl acetate/petroleum ether=1:5; silica gel: 200-300 mesh), which gives 10.5 g of 7-chloroquinoxalin-2-ylamine (yield 98%).

1. customThe mixture is then evaporated to dryness under reduced pressure
2. customAfter phase separation
3. washthe organic phase is then washed with 250 ml of water
4. dry with materialdried over sodium sulphate
5. customthe solvent is removed under membrane pump vacuum
6. customThe residue obtained
7. customis purified by column chromatography on silica gel (ethyl acetate/petroleum ether=1:5; silica gel: 200-300 mesh), which