Potassium Phosphate, Tribasic → HCID 90416585, compound

Participants

Reaction Steps

The product from Example 91D (1.233 g, 2.180 mmol), the product from Example 91C (0.8 g, 2.180 mmol), tris(dibenzylideneacetone)dipalladium(0) (0.060 g, 0.065 mmol), 1,3,5,7-tetramethyl-6-phenyl-2,4,8-trioxa-6-phosphaadamante (0.064 g, 0.218 mmol) and potassium phosphate (1.388 g, 6.54 mmol) were combined and sparged with argon for 15 minutes. Meanwhile a solution of 4:1 dioxane/water (18 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 ambient temperature, and partitioned between ethyl acetate and water. The organic layer was washed with saturated aqueous sodium chloride, dried (anhydrous Na2SO4), treated with 3-mercaptopropyl functionalized silica gel, filtered, and concentrated. Purification by chromatography (silica gel, 10-50% ethyl acetate in heptanes) afforded the title compound (0.104 g, 6%).

Provenance & Evidence