反应详情

温度

-70 °C

To a solution of 5-bromo-2-chloro-3-nitro-pyridine (7 g) in dry tetrahydrofuran (150 ml) at −70° C. under an atmosphere of nitrogen was added dropwise a solution of vinylmagnesium bromide (1.0M in tetrahydrofuran; 94.5 ml) over 1 h. The solution was stirred at −70° C. for 1 h and then quenched with saturated ammonium chloride (150 ml) and the aqueous was extracted twice with ethyl acetate. The combined organics were dried (MgSO4) and evaporated to give a deep red oil. The residue was triturated with diethyl ether (100 ml) and the solid was then filtered off, sucked dry then dried at 40° C. under vacuum to afford the title compound (1.75 g).

1. customquenched with saturated ammonium chloride (150 ml)
2. extractionthe aqueous was extracted twice with ethyl acetate
3. dry with materialThe combined organics were dried (MgSO4)
4. customevaporated
5. customto give a deep red oil
6. customThe residue was triturated with diethyl ether (100 ml)
7. filtrationthe solid was then filtered off
8. customsucked dry
9. customthen dried at 40° C. under vacuum