反应详情

To a solution of N-(3-trifluoromethylphenyl)-N'-cyano-O-phenylisourea (0.98 mmol, 286 mg) in dry acetonitrile (2 ml), isopropylamine (0.184 ml) and triethylamine (0.150 ml) were added. The mixture was stirred for 42 h at room temperature under nitrogen. After concentration the residue was purified by flash chromatography (ethyl acetate/heptane 1:2) to give the title compound (210 mg, 79%) as a syrup. Crystallization from ethyl acetate / heptane 1:3 gave white crystals (165 mg, 62%). Mp 109-111° C.; 1H-NMR (CDCl3): δ 1.20 (d, 6H), 4.05 (m,1H), 4.67 (br d, 1H), 7.42 (m, 1H), 7.50 (s,1H), 7.55 (m, 2H), 7.68 ppm (br, 1H); MA calc for C12H13F3N4 : C, 53.33%; H, 4.85%; N, 20.73%. Found: C, 53.61%; H, 4.92%; N, 20.67%.

1. concentrationAfter concentration the residue
2. customwas purified by flash chromatography (ethyl acetate/heptane 1:2)