反应详情

A mixture of 3-(4-{5-[5-(4-Methoxy-phenyl)-[1,3,4]oxadiazol-2-yl]-1H-benzoimidazol-2-yl}-3,5-dimethyl-phenyl)-2,2-dimethyl-propionic acid methyl ester (340 mg, 0.667 mmol) and aqueous 1M NaOH (5 mL, 5 mmol) in MeOH (5 mL) was stirred at room temperature for 18 h and then heated at 50° C. for 1 h. After the mixture was cooled to room temperature, the mixture was slowly acidified to pH 2˜3 by addition of 3M HCl. The product precipitated and was separated from the solution. The solid was dissolved in a small quantity of DMSO and purified by HPLC (basic) to give the title compound as a solid. 1H NMR (CD3OD, 400 MHz) δ ppm 8.55-8.45 (m, 1 H), 8.23 (d, J=8 Hz, 2 H), 8.22 (d, J=8 Hz, 1 H), 7.95-7.85 (m, 1 H), 7.26 (d, J=8 Hz, 2 H), 7.15 (s, 2 H), 4.02 (s, 3 H), 2.99 (s, 2 H), 2.26 (s, 6 H), 1.30 (s, 6 H). m/z 497.2 (MH+).

1. temperatureheated at 50° C. for 1 h
2. temperatureAfter the mixture was cooled to room temperature
3. customThe product precipitated
4. customwas separated from the solution
5. dissolutionThe solid was dissolved in a small quantity of DMSO
6. custompurified by HPLC (basic)