反应详情

温度

60 °C

The product from Example 311e (0.075 g, 0.198 mmol), the product from Example 6a (0.085 g, 0.198 mmol), tris(dibenzylideneacetone)dipalladium(0) (5.45 mg, 5.95 μmol), 1,3,5,7-tetramethyl-6-phenyl-2,4,8-trioxa-6-phosphaadamante (5.80 mg, 0.020 mmol) and potassium phosphate (0.126 g, 0.595 mmol) were combined and sparged with argon for 15 minutes. Meanwhile a solution of 4:1 dioxane/water (2 mL) was sparged with nitrogen for 15 minutes and transferred by syringe into the reaction vessel under argon. The mixture was stirred for 2 hours at 60° C. and partitioned between ethyl acetate and water. The organic layer was washed with saturated aqueous sodium chloride, dried (Na2SO4), treated with 3-mercaptopropyl functionalized silica gel, filtered, and concentrated. Purification by trituration in dichloromethane afforded the title compound (0.083 g, 70%).

1. customsparged with argon for 15 minutes
2. customMeanwhile a solution of 4:1 dioxane/water (2 mL) was sparged with nitrogen for 15 minutes
3. customtransferred by syringe into the reaction vessel under argon
4. custompartitioned between ethyl acetate and water
5. washThe organic layer was washed with saturated aqueous sodium chloride
6. dry with materialdried (Na2SO4)
7. additiontreated with 3-mercaptopropyl functionalized silica gel
8. filtrationfiltered
9. concentrationconcentrated
10. customPurification by trituration in dichloromethane