反应详情

2-Fluoro-4-nitrobenzoic acid (5 g, 27.01 mmol) was dissolved in acetonitrile (150 mL) and triethylamine (7.53 mL, 54.02 mmol). N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (7.8 g, 40.52 mmol) was added, followed by N-tert-butyl-3(piperazin-1-ylmethyl)benzamide (7.44 g, 27.01 mmol). The reaction was stirred at room temperature for 18 hours and concentrated under vacuum. The residue was dissolved in ethyl acetate, filtered through dicalite, washed consecutively with water (×2) and brine and concentrated under vacuum. The product was purified by strong cation exchange chromatography, eluting macroporous polystyrene sulfonic acid with 2M ammonia in methanol. The resulting solution was concentrated under vacuum to afford the title compound as a pale yellow oil (2.6 g). MS (ESI) m/z 443.7 [M+H]+

1. concentrationconcentrated under vacuum
2. dissolutionThe residue was dissolved in ethyl acetate
3. filtrationfiltered through dicalite
4. washwashed consecutively with water (×2) and brine
5. concentrationconcentrated under vacuum
6. customThe product was purified by strong cation exchange chromatography
7. washeluting macroporous polystyrene sulfonic acid with 2M ammonia in methanol
8. concentrationThe resulting solution was concentrated under vacuum