反应详情

温度

80 °C

A mixture of 1-[4-(4-Chloro-3-methoxy-phenyl)-piperazin-1-yl]-2-(3-iodo-pyrazolo[3,4-b]pyridin-1-yl)-ethanone (102.4 Mg), morpholine (0.20 mL), Xantphos (35 Mg), Pd2(dba)3 (18.3 Mg) and Cs2CO3 (97 Mg) in THF (1 mL) was heated to 80° C. for 12 h. The reaction mixture was allowed to cool to room temperature, diluted by EtOAc (3 mL) and filtered. The filtrate was evaporated in vacuo. The crude residue was purified by flash chromatography (silica, Hexane/EtOAc) to provide the title compound as a white powder: LCMS (ES) M+H 471.6, Rf 2.043 min (Agilent Zorbax SB-C18, 2.1×50 Mm, 5μ, 35° C., 1 mL/min flow rate, a 2.5 min gradient of 20% to 100% B with a 1.1 min wash at 100% B, A=0.1% formic acid/5% acetonitrile/94.9% water, B=0.1% formic acid/5% water/94.9% acetonitrile).

1. temperatureto cool to room temperature
2. filtrationfiltered
3. customThe filtrate was evaporated in vacuo
4. customThe crude residue was purified by flash chromatography (silica, Hexane/EtOAc)