反应详情

Heat a mixture of 2-chloro-5-nitro-3-trifluoromethyl-pyridine (2.27 g, 10 mmol), calcium chloride (1.1 g, 10 mmol) and iron powder (4.5 g) in ethanol (30 mL) and water (5 mL) at reflux for 1 hour. Cool the mixture and filter through Celite. Evaporate the filtrate, dissolve the residue in EtOAc (200 mL) and wash with saturated NaHCO3(aq) (100 mL) and brine (100 mL). Dry the organic extract over MgSO4 and remove the solvent under reduced pressure to yield the title compound.

1. temperatureHeat
2. temperatureat reflux for 1 hour
3. temperatureCool the mixture
4. filtrationfilter through Celite
5. customEvaporate the filtrate
6. dissolutiondissolve the residue in EtOAc (200 mL)
7. washwash with saturated NaHCO3(aq) (100 mL) and brine (100 mL)
8. customDry the
9. extractionorganic extract over MgSO4
10. customremove the solvent under reduced pressure