反应详情

温度

90 °C

A RBF was charged with (E)-ethyl 3-(2-amino-5-(benzylthio)phenyl)acrylate (2.0 g, 6.38 mmol)), 2,3-dichloro-5-iodo-6-methoxypyridine (2.327 g, 7.66 mmol)), xantphos (0.185 g, 0.319 mmol)), Pd2(dba)3 (0.146 g, 0.160 mmol)), and cesium carbonate (2.91 g, 8.93 mmol)) were added. A reflux condenser was attached and the flask was heated at 90° C. overnight. The mixture was cooled to RT, diluted with EtOAc, and filtered through celite, with the aid of EtOAc. The filtrate was concentrated and i-PrOH was added. The mixture was heated to 110° C. until all the material dissolved, then the solution was allowed to cool to RT overnight causing a yellow solid to crash out of solution. The solids were filtered and washed with i-PrOH, then dried under a nitrogen blanket to afford (E)-ethyl 3-(5-(benzylthio)-2-((5,6-dichloro-2-methoxypyridin-3-yl)amino)phenyl)acrylate (2.54 g, 5.19 mmol, 81% yield) as a yellow solid. m/z (ESI) 491.1 (M+H)+.

1. additionwere added
2. customA reflux condenser was attached
3. temperatureThe mixture was cooled to RT
4. filtrationfiltered through celite, with the aid of EtOAc
5. concentrationThe filtrate was concentrated
6. additioni-PrOH was added
7. temperatureThe mixture was heated to 110° C. until all the material
8. dissolutiondissolved
9. temperatureto cool to RT overnight
10. filtrationThe solids were filtered
11. washwashed with i-PrOH
12. customdried under a nitrogen blanket