反应详情

A solution of 1-(4-chloro-butyl)-5-methyl-4-pyridin-3-yl-1H-pyrimidin-2-one (Prep12, 86 mg, 0.31 mmol), (1S,5R)-1-(4-trifluoromethyl-phenyl)-3-aza-bicyclo[3.1.0]hexane (Prep4, 63 mg, 0.28 mmol), KI (2 mg) and K2CO3 (43 mg, 0.31 mmol) in DMF (2 ml) was placed in a microwave oven and irradiated at 115° C. for 1 hour. After cooling, the solution was diluted with water and extracted with ethyl acetate. The organic layer was washed with brine, dried (Na2SO4) and evaporated The solvent was removed under vacuum and the residue was redissolved in DCM and filtered, the filtrate was stirred in the presence of PS-isocyanate (350 mg) for 3 hours. The mixture was filtered and the solvent removed under vacuum. The crude was purified by flash chromatography with DCM-MeOH—NH4OH (99-1-0.1) to give the title compound (17 mg, 4% yield) as a free base.

1. customirradiated at 115° C. for 1 hour
2. temperatureAfter cooling
3. extractionextracted with ethyl acetate
4. washThe organic layer was washed with brine
5. dry with materialdried (Na2SO4)
6. customevaporated The solvent
7. customwas removed under vacuum
8. dissolutionthe residue was redissolved in DCM
9. filtrationfiltered
10. filtrationThe mixture was filtered
11. customthe solvent removed under vacuum
12. customThe crude was purified by flash chromatography with DCM-MeOH—NH4OH (99-1-0.1)