反应详情

温度

80 °C

To 6-Bromo-1-morpholinophthalazine (0.20 g, 680 μmol), 1,1′-bis(diphenylphosphino)ferrocene-palladium dichloride (50 mg, 68 μmol), potassium acetate (200 mg, 2040 μmol), and 4,4,5,5-tetramethyl-2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1,3,2-dioxaborolane (207 mg, 816 μmol) was added 1,4-dioxane (6.80 mL) and the mixture was heated to 80° C. for 2 h. The mixture was added to a sealed tube containing 4-chloro-3-iodobenzamide (230 mg, 816 μmol), tetrakis(triphenylphosphine)palladium (79 mg, 68 μmol), potassium carbonate—1.5 M in water (1.81 μl, 2.72 mmol), and ethanol (6.80 mL) and heated to 110° C. for 2 h. After cooling the reaction mixture was diluted with 75 mL of ethyl acetate, added to a separation funnel, partitioned with sodium bicarbonate (saturated, aqueous), washed 3 times with 50 mL of sodium bicarbonate (saturated, aqueous), separated, dried over sodium sulfate, concentrated in vacuo, and purified by HPLC to give the title compound.

1. additionThe mixture was added to a sealed tube
2. temperatureheated to 110° C. for 2 h
3. temperatureAfter cooling the reaction mixture
4. additionadded to a separation funnel
5. custompartitioned with sodium bicarbonate (saturated, aqueous)
6. washwashed 3 times with 50 mL of sodium bicarbonate (saturated, aqueous)
7. customseparated
8. dry with materialdried over sodium sulfate
9. concentrationconcentrated in vacuo
10. custompurified by HPLC