反应详情

After dissolving N1,4-dimethyl-5-bromo-2-ethoxybenzamide (200 g) in propionitrile (1.51), sodium cyanide (72 g), copper iodide (14 g) and tetrakis(triphenylphosphine)palladium (42 g) were added under a nitrogen atmosphere and the mixture was heated to reflux for 5 hours. Ethyl acetate and water were added and the reaction mixture was filtered through celite. The precipitated crystals in the filtrate were filtered off (15.4 g). This filtrate was then separated and washed with brine. The organic layer was dried over anhydrous magnesium sulfate and was concentrated after filtering off the insoluble portion. The obtained crystals were filtered off and washed with ethyl acetate (77.64 g). The crystals were combined to yield the title compound (93.04 g) as a white solid.

1. additionwere added under a nitrogen atmosphere
2. temperaturethe mixture was heated
3. temperatureto reflux for 5 hours
4. filtrationthe reaction mixture was filtered through celite
5. filtrationThe precipitated crystals in the filtrate were filtered off (15.4 g)
6. customThis filtrate was then separated
7. washwashed with brine
8. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
9. concentrationwas concentrated
10. filtrationafter filtering off the insoluble portion
11. filtrationThe obtained crystals were filtered off
12. washwashed with ethyl acetate (77.64 g)