反应详情

温度

150 °C

A 5 mL microwave vial was charged with Intermediate C (50 mg, 0.19 mmol), 2-(3,5-dichlorophenyl)-1H-imidazole (80 mg, 0.37 mmol), Pd2(dba)3 (35 mg, 0.04 mmol), BINAP (50 mg, 0.08 mmol), Cs2CO3 (120 mg, 0.37 mmol), and 2 mL of dioxane. The vial was sealed and heated in a microwave to 150° C. for 0.5 h. An additional 20 mg of Pd2(dba)3 was added, and the reaction mix was brought to 150° C. in the microwave again for 0.5 h to drive the reaction to completion. Upon cooling to 23° C., the reaction mix was diluted with EtOAc, and rinsed sequentially with saturated aqueous solutions of ammonium chloride, sodium bicarbonate, and brine. The resulting organic liquid was dried over sodium sulfate and decanted into a 250 mL round bottom flask. After concentration of the product under reduced pressure, the resulting residue was purified by HPLC (30-50% MeCN, 20 mL/min, 210 nM, 0.1% TFA. Stationary Phase: Phenomenex Luna C18, 2×25 cm) to give the title compound (19 mg). LCMS: 445.1 m/z (M+H)+; ret. Time: 4.20 min (Analytical Method C).

1. customThe vial was sealed
2. additionthe reaction mix
3. customthe reaction to completion
4. temperatureUpon cooling to 23° C.
5. additionthe reaction mix
6. washrinsed sequentially with saturated aqueous solutions of ammonium chloride, sodium bicarbonate, and brine
7. dry with materialThe resulting organic liquid was dried over sodium sulfate
8. customdecanted into a 250 mL round bottom flask
9. customAfter concentration of the product under reduced pressure, the resulting residue was purified by HPLC (30-50% MeCN, 20 mL/min, 210 nM, 0.1% TFA. Stationary Phase: Phenomenex Luna C18, 2×25 cm)