反应详情

温度

100 °C

Add methyl 2,6-dichloro-isonicotinate (2.06 g, 10.0 mmol), toluene (10 mL), tris(dibenzylideneacetone)dipalladium(0) (0.458 g, 0.50 mmol), 2-(di-tert-butylphosphino)biphenyl (0.298 g, 1.00 mmol), and methanesulfonamide sodium salt (1.17 g, 10.0 mmol) to a sealed flask flushed with nitrogen. Heat and stir the sealed flask at 100° C. for 18 h. Cool the mixture to room temperature and filter through a pad of filtering agent, and wash the solid with dichloromethane. Concentrate and purify (silica gel chromatography, eluting with 20:80 to 30:70 ethyl acetate:hexanes) to give the title compound (1.31 g, 50%).

1. customflushed with nitrogen
2. temperatureHeat
3. temperatureCool the mixture to room temperature
4. filtrationfilter through a pad
5. filtrationof filtering agent
6. washwash the solid with dichloromethane
7. concentrationConcentrate
8. custompurify
9. wash(silica gel chromatography, eluting with 20:80 to 30:70 ethyl acetate:hexanes)