反应详情

温度

90 °C

To a solution of the compound (135 mg, 0.42 mmol) prepared in Example 13, 3-methoxyphenylboronic acid (96 mg, 0.63 mmol), potassium phosphate (2N, 1 mL 2.0 mmol), tetrakis(triphenylphosphine)palladium(0) (Pd(PPh3)4) (11 mg, 0.01 mmol) in dioxane (3 mL) was deoxygenated by nitrogen gas for 5 minutes, and the reactor was sealed, heated at 90° C. for 20 hours. The mixture was concentrated, extracted with DCM and sodium hydroxide (1N). The organic layer was dried, concentrated, and the crude product was purified by prep TLC using 9% methanol in DCM (with 1% ammonium hydroxide) to obtain the title compound (98 mg) having the following physical data.

1. customthe reactor was sealed
2. concentrationThe mixture was concentrated
3. extractionextracted with DCM and sodium hydroxide (1N)
4. customThe organic layer was dried
5. concentrationconcentrated
6. customthe crude product was purified by prep TLC