反应详情

A mixture of chloropyrazine (10, 0.087 mol), 4-(trifluoromethyl)phenylboronic acid (21 g), palladium(diphenylphosphino)ferrocene dichloride (3.5 g, 5 mol %) and sodium carbonate (100 mL, 2M) in dioxane (200 mL) was degassed (×3) via Firestone valve. The mixture was heated under reflux for 1 h., evaporated in vacuo, the residue partitioned between ethyl acetate and water, then the organic phase was washed with brine, dried (MgSO4) and evaporated. The black residue was dry-loaded onto silica and purified by elution with 5-25% ethyl acetate in iso-hexane. This afforded the product as white crystals.

1. customwas degassed (×3) via Firestone valve
2. temperatureThe mixture was heated
3. temperatureunder reflux for 1 h.
4. customevaporated in vacuo
5. customthe residue partitioned between ethyl acetate and water
6. washthe organic phase was washed with brine
7. dry with materialdried (MgSO4)
8. customevaporated
9. custompurified by elution with 5-25% ethyl acetate in iso-hexane