反应详情

A mixture of 6-bromoisoquinoline (500 mg, 2.40 mmol) (commercially available from Kalexsyn Product List (Order Number 2003-005)), pyrazole-4-boronic acid pinacol ester (560 mg, 2.88 mmol) (commercially available from Acros Organics (Order Number 38294)), trans-dichlorobis(triphenylphosphine)palladium(II) (118 mg, 0.17 mmol), and sodium carbonate (764 mg, 7.21 mmol) in DME:EtOH:H2O=7:2:3 (4 mL) was heated at 140° C. for 10 minutes in a Biotage Initiator® microwave. After cooling to room temperature, the mixture was diluted with saturated aqueous NaHCO3 and extracted with 25% i-PrOH/CHCl3 (3×). The combined organic layers were dried over Na2SO4, filtered and adsorbed onto silica gel. The residue was purified using column chromatography (acetone/hexanes=0-50%) to provide the product as an off-white solid (177 mg, 37%). LCMS (API-ES) m/z: 196 (M+H+).

1. extractionextracted with 25% i-PrOH/CHCl3 (3×)
2. dry with materialThe combined organic layers were dried over Na2SO4
3. filtrationfiltered
4. customThe residue was purified