反应详情

Heat a solution of 1-(5-bromo-3-trifluoromethyl-pyridin-2-yl)-ethanone (268 mg, 1.0 mmol), zinc cyanide (75 mg, 0.63 mmol), pd2(dba)3 (30 mg), and DPPF (35 mg) in DMF (3 mL) and water (0.03 mL), under a nitrogen atmosphere, at 120° C. for 1 hour. Cool the reaction to 0° C. and add a solution of saturated ammonium chloride solution (2 mL), water (2 mL) and concentrated ammonium hydroxide (0.5 mL) and stir for 1 hour. Extract the mixture with ethyl acetate (3×20 mL) and wash the combined organics with brine (50 mL). Dry the organic extract over MgSO4 and remove the solvent under reduced pressure. Purify the residue by flash chromatography, eluting with a 9:1 mixture of hexane:ether to give the title compound.

1. temperatureCool
2. customthe reaction to 0° C.
3. extractionExtract the mixture with ethyl acetate (3×20 mL)
4. washwash the combined organics with brine (50 mL)
5. customDry the
6. extractionorganic extract over MgSO4
7. customremove the solvent under reduced pressure
8. customPurify the residue by flash chromatography
9. washeluting with a 9:1 mixture of hexane