反应详情

温度

0 °C

Dissolve 6-amino-3′-trifluoromethyl-[2,2′]bipyridinyl-5-carbonitrile (1.0 g, 7.6 mmol) in 12 N HCl (20 mL) and cool to 0° C. Add NaNO2 (731 mg, 10.6 mmol) in portions over the course of 15 minutes. Allow the mixture to stir for 1 hour at 0° C. Add CuCl (2.24 g, 22.7 mmol), allow the mixture to warm to room temperature and stir for 1 hour. Pour the mixture onto ice water (100 mL) and extract with EtOAc (3×100 mL);. Dry the combined organic extracts over Na2SO4 and remove the solvent under reduced pressure. Purify the crude product by silica gel chromatography eluting with EtOAc/hexane (1:1) to yield the title compound. MS 284.04 (M+1).

1. customover the course of 15 minutes
2. temperatureto warm to room temperature
3. stirringstir for 1 hour
4. additionPour the mixture onto ice water (100 mL)
5. extractionextract with EtOAc (3×100 mL)
6. dry with materialDry the combined organic extracts over Na2SO4
7. customremove the solvent under reduced pressure
8. customPurify the crude product by silica gel chromatography
9. washeluting with EtOAc/hexane (1:1)