反应详情

The crude residue from step 2 was dissolved in 22 mL dioxane and was treated with PdCl2(dppf)-CH2Cl2 adduct (0.608 g, 0.745 mmol), (2-methoxy-4-(trifluoromethyl)phenyl)boronic acid (1.802 g, 8.19 mmol), potassium carbonate (4.12 g, 29.8 mmol), and 8 mL water was added. The reaction mixture was allowed to stir at room temperature overnight. LC/MS showed product, so the aqueous layer was removed, and the reaction mixture was concentrated. Purification of the crude residue by silica gel column chromatography (0-50% EtOAc/heptane) gave 7-bromo-2-methoxy-4-(2-methoxy-4-(trifluoromethyl)phenyl)quinazoline (0.166 g, 0.402 mmol, 5.39% yield). (M+H)+=413.0.

1. additionwas added
2. customso the aqueous layer was removed
3. concentrationthe reaction mixture was concentrated
4. customPurification of the crude residue by silica gel column chromatography (0-50% EtOAc/heptane)