反应详情

温度

90 °C

A mixture of 8-bromo-6-chlorquinoline (140 mg, 0.56 mmol), (6-aminopyrdin-3-yl)(morpholino)methanone (92 mg, 0.44 mmol), xantphos (38.5 mg, 0.067 mmol) and cesium carbonate was taken up in dry dioxane (6.5 ml). The reaction flask is evacuated and back-filled with argon (repeated 5 times). Tris(dibenzylidenacetone)palladium (0) (31 mg, 0.033 mmol) was added and the flask was evacuated and back-filled with argon (repeated 3 times). The material was heated to 90° C. (oil bath) under argon for 14 hours. The reaction mixture was cooled to ambient temperature and filtered through a short plug of celite, rinsing well with dioxane. The solvent was removed and the resulting residue loaded onto 2 preparative thin layer chromatography plates. The plates were eluted with 75% ethyl acetate/hexane and the product band collected. This provided the desired product as a light brown viscous oil (180 mg).

1. customThe reaction flask is evacuated
2. additionback-filled with argon (repeated 5 times)
3. customthe flask was evacuated
4. additionback-filled with argon (repeated 3 times)
5. temperatureThe reaction mixture was cooled to ambient temperature
6. filtrationfiltered through a short plug of celite
7. washrinsing well with dioxane
8. customThe solvent was removed
9. washThe plates were eluted with 75% ethyl acetate/hexane
10. customthe product band collected