反应详情

6-Methyl-1-(4-piperidinyl)-5-(trifluoromethyl)-1,3-dihydro-2H-benzimidazol-2-one (free base of D60, 0.473 g, 1.47 mmol), 2-hydroxy-2-methylpropanenitrile (2 eq., 2.94 mmol, 0.268 ml), tetrahydro-4H-pyran-4-one (2 eq., 2.94 mmol, 0.27 ml), MgSO4 (880 mg) and N,N-dimethylacetamide (4 ml) were heated at 60° C. under argon for 24 hours. The mixture was subsequently cooled to room temperature and dichloromethane/water (70 ml/70 ml) were added and the biphasic mixture obtained was sonicated at room temperature for 20 minutes. The two phases were separated and the organic phase was dried by hydromatrix cartridge. The organic solvent was subsequently evaporated and the solid obtained was triturated with diethyl ether to afford the title compound (440 mgs, 70%).

1. customthe biphasic mixture obtained
2. customwas sonicated at room temperature for 20 minutes
3. customThe two phases were separated
4. customthe organic phase was dried by hydromatrix cartridge
5. customThe organic solvent was subsequently evaporated
6. customthe solid obtained
7. customwas triturated with diethyl ether