反应详情

温度

80 °C

To a stirred solution of the above Compound 19b (20 mg, 0.050 mmol), cyclohexylamine (11 μL, 0.13 mmol), and BINAP (4.7 mg, 0.0075 mmol) in toluene (0.4 mL) at 25° C. was added Pd2(dba)3 (2.3 mg, 0.0025 mmol) followed by NaOtBu (12 mg, 0.13 mmol). The solution was heated to 80° C. for 15 h. The solution was cooled, poured into H2O (5 mL), extracted with EtOAc (4×5 mL), dried (MgSO4), filtered and concentrated. HPLC (gradient elution, 90–10% H2O—CH3CN) provided the title compound (9.1 mg, 0.022 mmol, 44%).

1. temperatureThe solution was cooled
2. extractionextracted with EtOAc (4×5 mL)
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated
6. washHPLC (gradient elution, 90–10% H2O—CH3CN)