反应详情

温度

90 °C

To a stirred solution of 4-[5-(2-Amino-pyrimidin-5-yl)-1-tert-butyl-1H-benzoimidazol-2-yl]-3-[1,2,4]-triazol-1-yl-phenol (300 mg, 0.7 mmol) in DMF (10 mL) is added cesium carbonate (687 mg, 2.1 mmol) followed by Ethyl 3-chloro-2,2-dimethylpropanoate (231 mg, 1.4 mmol) at room temperature. The solution is heated to 90° C. for 72 hours. The solution is cooled to room temperature and is extracted with H2O (10 mL) and EtOAc (3×10 mL). The combined organic layer is dried with Mg2SO4 (500 mg) and is filtered. The filtrate is concentrated and the residue is purified by silica gel flash column chromatography with 10% MeOH in CH2Cl2 as the eluent to afford the title compound (200 mg, 51%). LCMS (ESMS): m/z: 555.40 (M++1).

1. temperatureThe solution is cooled to room temperature
2. extractionis extracted with H2O (10 mL) and EtOAc (3×10 mL)
3. dry with materialThe combined organic layer is dried with Mg2SO4 (500 mg)
4. filtrationis filtered
5. concentrationThe filtrate is concentrated
6. customthe residue is purified by silica gel flash column chromatography with 10% MeOH in CH2Cl2 as the eluent