反应详情

A solution of 2,3,5-trichlorobenzeneboronic acid (1.54 g, 6.82 mmol) in absolute ethanol (1.5 ml) was added slowly to a mixture of 2-amino-3-chloropyrazine (0.589 g, 4.54 mmol) and tetrakis(triphenylphosphine)palladium(0) (0.299 g, 0.259 mmol) in benzene (10.5 ml)/2M aqueous sodium carbonate (4.54 ml). The mixture was refluxed for 17 hours. The cooled reaction mixture was partitioned between water and ethylacetate (50 ml). The organic layer was washed with water (2×30 ml), dried (MgSO4) and evaporated. The crude product was purified by flash chromatography using chloroform to 0.5% methanol/chloroform as the eluent. The product was then crystallised from 40-60 petrol. Yield 0.15 g, 12% M.p. 142-143° C.

1. temperatureThe mixture was refluxed for 17 hours
2. customThe cooled reaction mixture
3. customwas partitioned between water and ethylacetate (50 ml)
4. washThe organic layer was washed with water (2×30 ml)
5. dry with materialdried (MgSO4)
6. customevaporated
7. customThe crude product was purified by flash chromatography
8. customThe product was then crystallised from 40-60 petrol