反应详情

Stirred dioxane (20 ml) at 80° C. was charged with 6-fluoro-2-iodo-3,4-dimethoxybenzonitrile from Example 1(a) (1.0 g, 3.3 mmol), tetrakis(triphenylphosphine)palladium(0) (0.19 g, 0.16 mmol), the pyridyl boronate from step (a) above (6.1 g, estimated to be 9.9 mmol), copper(I)iodide (0.25 g, 1.3 mmol), sodium carbonate (0.69 g, 6.5 mmol) and triphenylphosphine (0.17 g, 0.65 mmol) and the resulting brown slurry heated to reflux and stirred at this temperature overnight. The resulting suspension was cooled to room temperature, ethyl acetate (20 ml) and water (10 ml) added and the resulting mixture filtered through Arbocel™ filter aid. The phases were separated and the aqueous phase extracted with ethyl acetate (2×20 ml). The organic phases were combined, washed with saturated aqueous NaCl and stripped to an oil. Acetonitrile was added and the mixture warmed then cooled. The resulting suspension was filtered to give a solid that was dried in vacuo overnight at 45° C. to give 0.419 of the product (48%).

1. temperatureto reflux
2. filtrationthe resulting mixture filtered through Arbocel™
3. filtrationfilter aid
4. customThe phases were separated
5. extractionthe aqueous phase extracted with ethyl acetate (2×20 ml)
6. washwashed with saturated aqueous NaCl
7. additionAcetonitrile was added
8. temperaturethe mixture warmed
9. temperaturethen cooled
10. filtrationThe resulting suspension was filtered
11. customto give a solid
12. customthat was dried in vacuo overnight at 45° C.