反应详情

In a sealed tube under N2-atmosphere, N-(4-(4-chloropyrimidin-6-yl-oxy)-phenyl)-N′-(4-chloro-3-trifluoromethyl-phenyl)-urea (443 mg, 1.00 mmol) and 25% aqueous NH3 (2 ml) in ethanol (2 ml) is stirred for 22 h at 80° C. Then the reaction mixture is diluted with water and AcOEt, the aqueous layer separated off and extracted 3 times with AcOEt. The organic phases are washed with 3 portions of water and brine, dried (Na2SO4) and concentrated. Column chromatography (SiO2; CH2Cl2/MeOH 9:1) yields the title compound: m.p.: 197-198° C.; 1H-NMR (DMSO6): 9.20 (s, HN), 8.93 (s, HN), 8.12 (m, 1H), 8.08 (s, 1H), 7.63 (m, 2H), 7.51 (d, 2H), 7.08 (d, 2H), 6.82 (s, H2N), 5.67 (s, 1H).

1. customthe aqueous layer separated off
2. extractionextracted 3 times with AcOEt
3. washThe organic phases are washed with 3 portions of water and brine
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated