反应详情

A mixture 2,6-dichloropyrazine (0.671 mmol) and 3-picolylamine (2.014 mmol) in xylene (25 ml) was refluxed overnight. The residue obtained after evaporation of the solvent was suspended between CH2Cl2 (100 ml) and water (100 ml). The organic layer was separated and the aqueous layer was extracted with CH2Cl3 (3×50 ml). The combined organic extracts were washed with brine (1×100 ml), dried (Na2SO4) and the solvent removed in vacuo. The residue was then purified by column chromatography eluting with a hexane:ethyl acetate gradient mixture to afford the desired product (93%).

1. customThe residue obtained
2. customafter evaporation of the solvent
3. customThe organic layer was separated
4. extractionthe aqueous layer was extracted with CH2Cl3 (3×50 ml)
5. washThe combined organic extracts were washed with brine (1×100 ml)
6. dry with materialdried (Na2SO4)
7. customthe solvent removed in vacuo
8. customThe residue was then purified by column chromatography
9. washeluting with a hexane