反应详情

To a solution of 2,4-dioxo-1-(3-oxo-propyl)-1,2,3,4-tetrahydro-pyrimidine-5-carbonitrile (Prep35, 90 mg, 0.47 mmol) in dichloroethane (8 mL), (1S,5R)-1-(4-trifluoromethyl-phenyl)-3-aza-bicyclo[3.1.0]hexane (Prep4, 106 mg, 0.47 mmol), AcOH (42 mg, 0.7 mmol) and NaBH(AcO)3 (198 mg, 0.94 mmol) were added and the mixture was stirred at room temperature overnight. The solvent was evaporated under vacuum, the residue redissolved in ethyl acetate and the obtained mixture washed with aqueous saturated NaHCO3 solution. The organic phase was dried (Na2SO4) and evaporated. The crude was purified by flash chromatography with DCM-MeOH—NH4OH (97-3-1) to give the free base of the title compound as a white solid (70 mg, 38% yield).

1. customThe solvent was evaporated under vacuum
2. dissolutionthe residue redissolved in ethyl acetate
3. washthe obtained mixture washed with aqueous saturated NaHCO3 solution
4. dry with materialThe organic phase was dried (Na2SO4)
5. customevaporated
6. customThe crude was purified by flash chromatography with DCM-MeOH—NH4OH (97-3-1)