反应详情

A mixture of dimethyl 4-aminobenzylphosphonate (0.86 g), (2E)-3-[5-(4-fluorophenyl)-1-methyl-1H-pyrazol-4-yl]acrylic acid (0.74 g), 1-hydroxy-1H-1,2,3-benzotriazole hydrate (0.61 g), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (0.77 g) and N,N-dimethylfomamide (8 ml) was stirred at room temperature overnight. The reaction mixture was poured into a 0.5N aqueous hydrochloric acid solution and extracted with ethyl acetate. The ethyl acetate layer was washed with saturated aqueous sodium hydrogen carbonate, and then with saturated brine, dried (MgSO4) and concentrated. The obtained solid was recrystallized from acetone-water to give (2E)-N-[4-(dimethylphosphonomethyl)phenyl]-3-[5-(4-fluorophenyl)-1-methyl-1H-pyrazol-4-yl]acrylamide (0.86 g, yield 65%) as colorless prism crystals. melting point: 209-210° C.

1. extractionextracted with ethyl acetate
2. washThe ethyl acetate layer was washed with saturated aqueous sodium hydrogen carbonate
3. dry with materialwith saturated brine, dried (MgSO4)
4. concentrationconcentrated
5. customThe obtained solid was recrystallized from acetone-water