反应详情

温度

80 °C

To a solution of 7-Chloro-3-iodo-imidazo[1,2-a]pyridine (15.17 g, 54.5 mmol) in 1,4-dioxane (260 ml) was added 1-[3-(4,4,5,5-Tetramethyl-[1,3,2]dioxaborolan-2-yl)-phenyl]-3-(2,2,2-trifluoro-ethyl)-urea (22.5 g, 65.4 mmol) and aqueous K3PO4 (23.1 g in 65 ml H2O, 109 mmol) [reaction degassed by bubbling N2 through] followed by 1,1′-bis(diphenylphosphino)ferrocene palladium (II) chloride (1.99 g, 2.72 mmol). The mixture was heated at 80° C. overnight, then diluted with water and extracted with EtOAc. The organic layer was washed with brine, dried (MgSO4), filtered and concentrated under reduced pressure. The residue was triturated with DCM (100 ml), filtered and the filtercake washed with 1:1 DCM:Petroleum ether to give the product (13.2 g) as a beige solid. MS: [M+H]+=369.

1. extractionextracted with EtOAc
2. washThe organic layer was washed with brine
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe residue was triturated with DCM (100 ml)
7. filtrationfiltered
8. washthe filtercake washed with 1:1 DCM