反应详情

温度

80 °C

A mixture of 10-(benzyloxy)-4-bromo-2-(4-fluorobenzyl)-8-methyl-7,8-dihydropyrazino[1′,2′:1,5]pyrrolo[2,3-d]pyridazine-1,9(2H,6H)-dione (0.10 g, 0.19 mmol; Example 160, step 1), pyrimidine-5-boronic acid (73 mg, 0.59 mmol), cesium fluoride (0.12 g, 0.78 mmol), bis(tri-t-butylphosphine)palladium(0) (10 mg, 0.02 mmol), and tris(dibenzylideneacetone)dipalladium (18 mg, 0.02 mmol) in dioxane (3 mL) was purged with nitrogen for 2 minutes and heated in a sealed tube at 80° C. overnight. The reaction mixture was filtered through a pad of Celite, and the filtrate was concentrated under vacuum. The residue was subjected to column chromatography on silica gel eluting with 0 to 20% methanol in chloroform gradient. Collection and concentration of appropriate fractions afforded the title material.

1. customwas purged with nitrogen for 2 minutes
2. filtrationThe reaction mixture was filtered through a pad of Celite
3. concentrationthe filtrate was concentrated under vacuum
4. customCollection and concentration of appropriate fractions