反应详情

温度

170 °C

A mixture of 17 (110 mg, 0.297 mmol), Zn(CN)2 (71 mg, 0.594 mmol, 2 equiv), [(t-Bu)3P]2 Pd (0.78 g, 0.149 mmol, 0.5 equiv) and Zn powder (29 mg, 0.446 mmol, 1.5 eq) were suspended in anhydrous NMP and degassed. The reaction mixture was heated to 170° C. for 30 h. After cooling to 25° C., the reaction was quenched with 2 N NH4OH (20 mL) and extracted with EtOAc (2×25 mL). The combined organic phases were washed with brine, dried (MgSO4) and concentrated. Chromatography (SiO2, 50 to 60% EtOAc-hexane) afforded the desired product as an off-white solid (49 mg, 46%). mp >280° C. ESI HRMS m/z 361.1293 (M++H, C18H16F3N4O requires 361.1276).

1. customdegassed
2. temperatureAfter cooling to 25° C.
3. customthe reaction was quenched with 2 N NH4OH (20 mL)
4. extractionextracted with EtOAc (2×25 mL)
5. washThe combined organic phases were washed with brine
6. dry with materialdried (MgSO4)
7. concentrationconcentrated