反应详情

4-Amino-N-{2-[4-(4-fluorobenzoyl)piperidino]ethyl}-N-(4-methoxyphenyl)benzamide (237.0 mg, 0.50 mmol) was dissolved in acetic acid (5.0 ml), and the solution was mixed with 2,5-dimethoxytetrahydrofuran (0.065 ml, 0.50 mmol) and heated for 1 hour under reflux. After cooling, acetic acid was distilled off under a reduced pressure, the residue was dissolved in ethyl acetate, and the organic layer was washed with water and saturated brine, and dried on anhydrous sodium sulfate. Thereafter, the solvent was distilled off under a reduced pressure, and the resulting residue was purified by a silica gel column chromatography (hexane:ethyl acetate=1:4) to obtain 217.0 mg (82,7%) of the title compound in a colorless amorphous form.

1. temperatureheated for 1 hour
2. temperatureunder reflux
3. temperatureAfter cooling
4. distillationacetic acid was distilled off under a reduced pressure
5. dissolutionthe residue was dissolved in ethyl acetate
6. washthe organic layer was washed with water and saturated brine
7. dry with materialdried on anhydrous sodium sulfate
8. distillationThereafter, the solvent was distilled off under a reduced pressure
9. customthe resulting residue was purified by a silica gel column chromatography (hexane:ethyl acetate=1:4)