反应详情

6-Bromo-1-morpholinophthalazine (191 mg, 649 μmol), 4-methyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoic acid (170 mg, 649 μmol), and tetrakis (triphenylphosphine)palladium (75 mg, 65 μmol) were added to a microwave vial before sodium carbonate-2 N in water (1.9 mL, 3892 μmol) and ethanol (3.2 mL) were added. The reaction mixture was reacted in a microwave oven for 10 min at 160° C. The reaction was cooled, diluted with 50 mL of EtOAc, added to an addition funnel and partitioned with sodium bicarbonate (saturated, aqueous). The organic layer was washed 2 times with 50 mL of sodium bicarbonate (saturated, aqueous), and separated. The aqueous layer was acidified to pH 5 with conc. HCl and extracted 4 times with 50 mL of chloroform. The organic layers were combined, dried over sodium sulfate, and concentrated via rotovap to give the title compound. Found MS (ES+): 350 (M+H)+.

1. additionwere added
2. customThe reaction mixture was reacted in a microwave oven for 10 min at 160° C
3. temperatureThe reaction was cooled
4. additionadded to an addition funnel
5. custompartitioned with sodium bicarbonate (saturated, aqueous)
6. washThe organic layer was washed 2 times with 50 mL of sodium bicarbonate (saturated, aqueous)
7. customseparated
8. extractionextracted 4 times with 50 mL of chloroform
9. dry with materialdried over sodium sulfate
10. concentrationconcentrated via rotovap