反应详情

N-(1-benzyl-4-piperidinyl)-2,2,2-trifluoroacetamide (1.0 g, 3.49 mmol) was added to a suspension of 60%-sodium hydride (147 mg, 3.67 mmol) in tetrahydrofuran (20 ml) at room temperature and stirred for 30 minutes. Then, methyl iodide (0.239 ml, 3.84 mmol) was added thereto and stirred for 5 hours. The reaction solution was poured into water and extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate and distilled under reduced pressure to remove the solvent, and the resulting residue was purified by a silica gel column chromatography (eluent: chloroform/methanol=100/1) to obtain N-(1-benzyl-4-piperidinyl)-2,2,2-trifluoro-N-methylacetamide (731 mg, 70%).

1. stirringstirred for 5 hours
2. extractionextracted with ethyl acetate
3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
4. distillationdistilled under reduced pressure
5. customto remove the solvent
6. customthe resulting residue was purified by a silica gel column chromatography (eluent: chloroform/methanol=100/1)