反应详情

Load in a 5 mL septum capped vial the following: small magnetic stir bar, 1-[4-(7-chloro-imidazo[1,2-a]pyridin-3-yl)-phenyl]-3-(3-trifluoromethyl-phenyl)-urea (250 mg, 0.58 mmol), 4-pyridyl boronic acid (77.4 mg, 0.63 mmols, 1.1 Eq), S-phos (236 mg), Pd(OAc)2 (60 mg), K3PO4 (237 mg, 1.12 mmol), 1,4-dioxane: H2O 2:1. Heat the reaction to 50° C. for 24 hours, cool and purify with a Varian SCX® (10 g) column that is pre-washed with water and methanol, and elute the product with 2 N NH3 in methanol. Evaporate the product containing fractions under reduced pressure and take up into CH2Cl2 and chromatograph using SiO2 eluting with a gradient of 0% to 10% of 2 M NH3 in MeOH with the balance CH2Cl2. Evaporate the fractions containing the product under reduced pressure, then vacuum oven dry at 40° C. to give the title compound as a yellow solid 61.8 mg (22.5%). MS (ES), m/z 474 (M+1).

1. temperatureHeat
2. customthe reaction to 50° C. for 24 hours
3. temperaturecool
4. custompurify with a Varian SCX® (10 g) column that
5. washis pre-washed with water and methanol
6. washelute the product with 2 N NH3 in methanol
7. customEvaporate the product
8. additioncontaining fractions under reduced pressure
9. customEvaporate the fractions
10. additioncontaining the product under reduced pressure
11. customvacuum oven dry at 40° C.