反应详情

温度

0 °C

A solution of 3-[5-(2-chloro-pyridin-3-yl)-2,4-dioxo-3,4-dihydro-2H-pyrimidin-1-yl]-propionaldehyde (Prep97, 128 mg, 0.46 mmol), (1S,5R)-1-(4-trifluoromethyl-phenyl)-3-aza-bicyclo[3.1.0]hexane (Prep4, 104 mg, 0.46 mmol), and AcOH (32 μl) in dichloroethane-MeOH (10-01, 4 ml) was cooled to 0° C. NaBH(AcO)3 (102 mg, 0.48 mmol) was added portionwise. The mixture was stirred at 0° C. for further 1 hour and then basified with 1N NaOH. The product was extracted with DCM. The organic phase was dried (Na2SO4) and evaporated. The crude was purified by flash chromatography eluting with DCM-MeOH—NH4OH (98:2:0.2) to give 77 mg of the free base of title compound (34% yield).

1. extractionThe product was extracted with DCM
2. dry with materialThe organic phase was dried (Na2SO4)
3. customevaporated
4. customThe crude was purified by flash chromatography
5. washeluting with DCM-MeOH—NH4OH (98:2:0.2)