反应详情

温度

100 °C

A mixture of (R)-8-bromo-6-(4-chlorophenyl)-1,4-dimethyl-5,6-dihydro-4H-benzo[b][1,2,4]triazolo[4,3-d][1,4]diazepine (41 mg, 0.1 mmol), 1,5-dimethyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole (34 mg, 0.15 mmol), tetrakis(triphenylphosphine)palladium(0) (12 mg) and cesium carbonate (65 mg, 0.2 mmol) in toluene, ethanol and water (5 mL, 4:2:1) was stirred at 100° C. for 0.5 hour under microwave (pressure: 3.2 bar, equipment power: 150 W). The reaction mixture was evaporated, water (10 mL) was added and the mixture was extracted with ethyl acetate (20 mL). The combined organic layers were dried over anhydrous sodium sulfate, filtered and concentrated to give a residue which was purified by column chromatography (silica gel, petroleum ether/ethyl acetate=2:1), to give (R)-6-(4-chlorophenyl)-8-(1,5-dimethyl-1H-pyrazol-4-yl)-1,4-dimethyl-5,6-dihydro-4H-benzo[b][1,2,4]triazolo[4,3-d][1,4]diazepine as a yellow solid (10 mg, 23%).

1. customThe reaction mixture was evaporated
2. additionwater (10 mL) was added
3. extractionthe mixture was extracted with ethyl acetate (20 mL)
4. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customto give a residue which
8. customwas purified by column chromatography (silica gel, petroleum ether/ethyl acetate=2:1)