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温度

0 °C

3-((4-(4-Aminobenzoyl)piperazin-1-yl)methyl)-N-tert-butylbenzamide (0.203 mmol, 0.080 g) and triethylamine (1.015 mmol, 0.103 g) were dissolved in dichloromethane (12 mL) and the stirred mixture was cooled to 0° C. Benzoyl chloride (0.305 mmol, 0.043 g) was added and the reaction mixture was allowed to reach room temperature and stir overnight. Water was added to the reaction and the organic layer was then separated, dried (sodium sulfate) and concentrated under vacuum. The residue was purified by silica column chromatography (dichloromethane/methanol (5% to 10%)) and coevaporated with dichloromethane (×3) and diethyl ether (×3) to give the title compound (93 mg). MS (ESI) m/z 499.8 [M+H]+

1. customto reach room temperature
2. customthe organic layer was then separated
3. dry with materialdried (sodium sulfate)
4. concentrationconcentrated under vacuum
5. customThe residue was purified by silica column chromatography (dichloromethane/methanol (5% to 10%))