反应详情

温度

0 °C

3-[5-(3-Fluoro-pyridin-4-yl)-2,4-dioxo-3,4-dihydro-2H-pyrimidin-1-yl]-propionaldehyde (Prep69, 63 mg, 0.24 mmol) was dissolved in DCM-MeOH 1-1 (2 ml). The resulting solution was cooled at 0° C. and then (1S,5R)-1-(4-trifluoromethyl-phenyl)-3-aza-bicyclo[3.1.0]hexane (54 mg, 0.24 mmol), AcOH (17 μl) and NaBH(AcO)3 (55 mg, 0.26 mmol) were added. The mixture was left to reach room temperature and the stirring was prolonged for further 18 hours. 1N NaOH was added and the product was extracted with DCM. The organic phase was dried (Na2SO4) and evaporated. The crude was redissolved in DCM and treated with PS-isocyanate (300 mg) overnight. The residue was finally purified with SCX cartridge, washing with MeOH and then collecting the product with MeOH—NH4OH (95-5) to give 17 mg of the title compound (16% yield).

1. waitThe mixture was left
2. customto reach room temperature
3. extractionthe product was extracted with DCM
4. dry with materialThe organic phase was dried (Na2SO4)
5. customevaporated
6. dissolutionThe crude was redissolved in DCM
7. additiontreated with PS-isocyanate (300 mg) overnight
8. customThe residue was finally purified with SCX cartridge
9. washwashing with MeOH
10. customcollecting the product with MeOH—NH4OH (95-5)