反应详情

Heat a mixture of 6-chloro-5-trifluoromethyl-pyridin-3-ylamine (985 mg, 5.0 mmol), palladium acetate (20 mg), DPPP (60 mg), butyl vinyl ether (1.5 g, 15 mmol) and NaHCO3 (840 mg, 10 mmol) in MeOH (10 mL) at 130° C. for 18 hours. Cool, filter and wash the solid with MeOH. Add 6M hydrochloric acid (5 mL), stir for 1 hour and evaporate the volatiles. Dissolve the residue in EtOAc (50 mL) and wash with saturated NaHCO3(aq) (50 mL) and brine (50 mL). Dry the organic extract over MgSO4 and remove the solvent under reduced pressure to yield the title compound.

1. temperatureHeat
2. temperatureCool
3. filtrationfilter
4. washwash the solid with MeOH
5. additionAdd 6M hydrochloric acid (5 mL)
6. customevaporate the volatiles
7. dissolutionDissolve the residue in EtOAc (50 mL)
8. washwash with saturated NaHCO3(aq) (50 mL) and brine (50 mL)
9. customDry the
10. extractionorganic extract over MgSO4
11. customremove the solvent under reduced pressure