反应详情

Diethylaminosulfur trifluoride (57 μL) is added drop wise to N-cyclopropyl-N-[1-(2-hydroxy-2-methyl-propyl)-piperidin-4-yl]-4-oxazol-5-yl-benzamide (83 mg) in dry dichloromethane (12 mL) at −78° C. and the reaction mixture is stirred at this temperature for 2 h. The mixture is poured on aqueous NaHCO3 solution (15 mL) and the aqueous phase is extracted with dichloromethane. The combined extracts are washed with brine, dried over MgSO4 and concentrated in vacuo. The solid residue is triturated with diisopropyl ether, filtered off, and dried to give the title compound. LC (method 2): tR=1.10 min; Mass spectrum (ESI+): m/z =386 [M+H]+.

1. extractionthe aqueous phase is extracted with dichloromethane
2. washThe combined extracts are washed with brine
3. dry with materialdried over MgSO4
4. concentrationconcentrated in vacuo
5. customThe solid residue is triturated with diisopropyl ether
6. filtrationfiltered off
7. customdried