反应详情

温度

65 °C

A mixture of methyl 3-chloro-4-((5-(2-(3,4-dichlorophenyl)propan-2-yl)-1-(4-fluorophenyl)-1H-imidazol-2-yl)methoxy)-5-fluorobenzoate (120 mg, 0.21 mmol) and 2N NaOH (0.31 mL, 0.63 mmol) in MeOH (3 mL) was heated 3 h at 65° C. After cooling, the reaction was neutralized to pH 3 with 3N HCl, concentrated under reduced pressure, diluted with water, and then extracted with EtOAc. The combined extracts were washed with brine, dried over Na2SO4, and concentrated in vacuo. The crude material was purified by HPLC (MeCN/H2O, 10-99%) to give the title compound as an off-white solid (45 mg, 39%). MS (EI) m/z 553.5 [M+H]+.

1. temperatureAfter cooling
2. concentrationconcentrated under reduced pressure
3. additiondiluted with water
4. extractionextracted with EtOAc
5. washThe combined extracts were washed with brine
6. dry with materialdried over Na2SO4
7. concentrationconcentrated in vacuo
8. customThe crude material was purified by HPLC (MeCN/H2O, 10-99%)