反应详情

温度

90 °C

A mixture of 6-bromo-1-(ethylthio)phthalazine (1.87 g), N-cyclopropyl-4-methyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzamide (0.3 g, 0.9 mmol), and tetrakis(triphenylphosphine) palladium(0) (0.05 g, 0.05 mmol) in DME/EtOH (4:1) (5 mL) was treated with the 2 M aqueous solution of potassium carbonate (1 mL, 3 mmol). The mixture was heated at 90° C. for 1 h. The mixture was cooled, diluted with ethyl acetate (100 mL), washed with water (3×20 mL), brine 20 mL, dried over anhydrous Na2SO4, and concentrated in vacuo. The crude product was purified by chromatography eluting with 1-5% 2 M ammonia methanol/dichloromethane to give the title compound as pale yellow solid. Found MS(ES+): 364(M+H)+.

1. temperatureThe mixture was cooled
2. washwashed with water (3×20 mL), brine 20 mL
3. dry with materialdried over anhydrous Na2SO4
4. concentrationconcentrated in vacuo
5. customThe crude product was purified by chromatography
6. washeluting with 1-5% 2 M ammonia methanol/dichloromethane