反应详情

To a solution of 1-(cyclopropylmethyl)-3-(4-(piperazine-1-carbonyl)phenyl)urea (1.654 mmol, 500 mg), 4-(1,1,1,3,3,3-hexafluoro-2-hydroxypropan-2-yl)benzoic acid (1.654 mmol, 476 mg) and triethylamine (4.96 mmol, 0.691 mL, 502 mg) in dichloromethane (50 mL) was added 1-propanephosphonic acid cyclic anhydride (2.480 mmol, 0.738 mL, 789 mg; 50% solution in ethyl acetate). The reaction mixture was stirred for 2 hours then was diluted with ethyl acetate and sodium carbonate (aqueous). The organic layer was separated, dried (magnesium carbonate) and concentrated under reduced pressure. The residue was chromatographed on silica eluting with a gradient of dichloromethane to ethyl acetate to give the title compound (180 mg). MS (ESI) m/z 571.0 [M−H]−

1. customThe organic layer was separated
2. dry with materialdried (magnesium carbonate)
3. concentrationconcentrated under reduced pressure
4. customThe residue was chromatographed on silica eluting with a gradient of dichloromethane to ethyl acetate