反应详情

温度

110 °C

In a microwave vial are added N1-tert-Butyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-benzene-1,2-diamine (100 mg, 0.5 mmol) and 5-bromo-2,3-dihydro-1H-pyrrolo[2,3-b]pyridine (180 mg, 0.62 mmol), tetrakis(triphenylphosphine)palladium(0) (58 mg, 0.05 mmol) and K2CO3 (139 mg, 1 mmol) in DMF (4 mL) and H2O (0.2 mL). The reaction mixture is heated at 110° C. in a microwave reactor for 1 hour. The reaction is cooled down to room temperature, poured into H2O (10 mL) and extracted with EtOAc (3×10 mL). The combined organic layer is dried (MgSO4), filtered and concentrated. The residue is purified by silica gel flash column chromatography eluting with 10% MeOH in CH2Cl2 to afford the title intermediate (40 mg, 28%). LCMS (ESMS): m/z 283.20 (M++1)

1. temperatureThe reaction is cooled down to room temperature
2. extractionextracted with EtOAc (3×10 mL)
3. dry with materialThe combined organic layer is dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue is purified by silica gel flash column chromatography
7. washeluting with 10% MeOH in CH2Cl2