反应详情

To 4-amino-2-chloro-3-fluorobenzoic acid (2.64 mmol, 500 mg) and N-tert-butyl-3-(piperazin-1-ylmethyl)benzamide (2.54 mmol, 700 mg) and triethylamine (10.76 mmol, 1.5 mL, 1089 mg) in dichloromethane (30 mL) was added 1-propanephosphonic acid cyclic anhydride (6.75 mmol, 4 mL, 4296 mg, 50% solution in ethyl acetate). After 2 hours stirring, ethyl acetate was added. The organic mixture was washed with saturated sodium hydrogen carbonate, water, and saturated sodium chloride. The organic mixture was dried sodium sulfate, filtered and concentrated under reduced pressure. The crude residue was purified by silica chromatography (eluting with 5% methanol in dichloromethane) to yield the title compound (325 mg). MS (ESI) m/z 447.1 [M+H]+

1. washThe organic mixture was washed with saturated sodium hydrogen carbonate, water, and saturated sodium chloride
2. filtrationfiltered
3. concentrationconcentrated under reduced pressure
4. customThe crude residue was purified by silica chromatography (eluting with 5% methanol in dichloromethane)