反应详情

A mixture of palladium (II) acetate (830 mg, 3.7 mmole), 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (3.46 g, 5.5 mmole) and cesium carbonate (18.1 g, 56 mmole) in dry degassed 1,4-dioxane (200 ml) under argon was sonicated at 28° C. for 0.5 h producing a pink heterogeneous mixture. This was treated with D1 (10 g, 37 mmole) followed by cis-2,6-dimethylpiperazine (12.6 g, 110 mmole) and heated with rapid stirring at reflux for 96 h. The mixture was allowed to cool, filtered through Kieselguhr and then concentrated under vacuum. The residue was treated with EtOAc and 2M HCl acid, shaken well and the aqueous layer separated, basified by addition of K2CO3 and extracted with DCM. The extract was dried (Na2SO4) and concentrated under vacuum to afford the title compound as a pale orange solid (7.1 g, 63%). MH+ 304.

1. customin dry
2. customdegassed 1,4-dioxane (200 ml) under argon
3. customwas sonicated at 28° C. for 0.5 h
4. customproducing a pink heterogeneous mixture
5. temperatureheated
6. temperatureat reflux for 96 h
7. temperatureto cool
8. filtrationfiltered through Kieselguhr
9. concentrationconcentrated under vacuum
10. additionThe residue was treated with EtOAc and 2M HCl acid
11. stirringshaken well
12. customthe aqueous layer separated
13. additionbasified by addition of K2CO3
14. extractionextracted with DCM
15. dry with materialThe extract was dried (Na2SO4)
16. concentrationconcentrated under vacuum