反应详情

温度

40 °C

Load a 5 mL septum capped vial with the following: small magnetic stir bar, 1-[4-(7-chloro-imidazo[1,2-a]pyridin-3-yl)-benzyl]-3-(3-trifluoromethyl-phenyl)-urea (208 mg, 0.46 mmol), 6-methoxy-pyridin-3-yl boronic acid (0.51 mmols, 1.1 Eq), 2-dicyclohexylphosphino-2′,6′-dimethoxy-1,1′-biphenyl (23.6 mg), Pd(OAc)2 (5 mg), K3PO4 (218 mg, 1.03 mmol), dioxane:H2O 2:1 (3 mL). Deoxygenate the reaction with N2 and heat to 40° C. for 24 hours. Cool the mixture and pour into a separatory funnel containing CH2Cl2 (45 mL) and H2O (2 mL). Extract the CH2Cl2 and evaporate under reduced pressure. Mix the residue with CH2Cl2 and a small amount of acetone. Filter the resulting solid and rinse with a small amount of CH2Cl2 and air dry. Vacuum oven dry the solid at 40° C. to give the title compound in 56% yield: MS(ES), m/z 518 (M+1).

1. customDeoxygenate
2. customthe reaction with N2
3. temperatureCool the mixture
4. additionpour into a separatory funnel
5. extractionExtract the CH2Cl2
6. customevaporate under reduced pressure
7. additionMix the residue with CH2Cl2
8. filtrationFilter the resulting solid
9. washrinse with a small amount of CH2Cl2 and air
10. customdry
11. customVacuum oven dry the solid at 40° C.