反应详情

2-Bromo-5-chloropyridine (13.42 g, 0.067 mol), tris(dibenzylideneacetone)-dipalladium(0) (1.32 g, 1.43 mmol), sodium tert-butoxide (8.55 g, 0.088 mol), capped with a septum and purged with N2. A mixture of 4-methoxy-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine (9.55 g, 0.0549 mol) in dry nitrogen-sparged toluene was added and the reaction mixture was sparged with nitrogen for an additional 30 min. The reaction mixture was then planced in an oil bath at 100° C., and heated overnight. After cooling, the mixture was diluted with ethyl acetate (180 mL), filtered and concentrated in vacuo. The residue was absorbed on 43 g silica, and purified on silica gel columned (0-60% EtOAc/hexane) to afford a light orange solid.

1. custompurged with N2
2. customsparged toluene
3. additionwas added
4. customthe reaction mixture was sparged with nitrogen for an additional 30 min
5. customThe reaction mixture was then planced in an oil bath at 100° C.
6. temperatureheated overnight
7. temperatureAfter cooling
8. additionthe mixture was diluted with ethyl acetate (180 mL)
9. filtrationfiltered
10. concentrationconcentrated in vacuo
11. customThe residue was absorbed on 43 g silica
12. custompurified on silica gel
13. customto afford a light orange solid