反应详情

温度

73 °C

A suspension of 1-[4-(3-chloro-4-cyanoisothiazol-5-yl)phenyl]-3-(2-fluoro-5-methylphenyl)urea (4.3 g, 11.1 mmol) in 15 mL of 2,4-dimethoxybenzylamine was heated to 73° C. for 24 h. The reaction became clear after ˜3 h. The reaction was cooled to RT. The residue was diluted with 300 mL of DCM and was washed with 10% HCl solution two times, saturated Na2S2O5 two times followed by brine. The organic solution was dried with MgSO4, filtered, and concentrated. The crude product was purified by flash silica gel column eluted with 2-5% MTBE in DCM/hexanes (2:1) to obtain the title compound as a light yellow solid (1.19 g, 21%).

1. temperatureThe reaction was cooled to RT
2. washwas washed with 10% HCl solution two times, saturated Na2S2O5 two times
3. dry with materialThe organic solution was dried with MgSO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe crude product was purified by flash silica gel column
7. washeluted with 2-5% MTBE in DCM/hexanes (2:1)