反应详情

A solution of 1-(4-{(1S,5R)-1-[4-(trifluoromethyl)phenyl]-3-azabicyclo[3.1.0]hex-3-yl}butyl)-2,4(1H,3H)-pyrimidinedione (E5, 110 mg, 0.3 mmol) and Lawesson's reagent (184 mg, 0.5 mmol) in DME (2 mL) was stirred at reflux for 2 hours. The solvent was evaporated under vacuum. The crude was re-dissolved in ethyl acetate and washed with water. The organic phase was dried (Na2SO4) filtered and evaporated; the crude was purified by flash chromatography with DCM-MeOH—NH4OH (98-2-0.2) to give the title compound as a yellow oil (80 mg, 63% yield).

1. temperatureat reflux for 2 hours
2. customThe solvent was evaporated under vacuum
3. dissolutionThe crude was re-dissolved in ethyl acetate
4. washwashed with water
5. dry with materialThe organic phase was dried (Na2SO4)
6. filtrationfiltered
7. customevaporated
8. customthe crude was purified by flash chromatography with DCM-MeOH—NH4OH (98-2-0.2)