反应详情

温度

80 °C

To the resulting 5,6-dimethylbenzimidazole-2-thiol (89 mg, 0.50 mmol) in dimethylformamide (2 ml), triethylamine (84 μl, 0.6 mmol) and 2-bromomethyl benzoic acid methyl ester (137 mg, 0.6 mmol) were added. After the resulting solution was stirred at 80° C. for 1.5 hours, water was added, followed by extraction with ethyl acetate. After drying the ethyl acetate phase with anhydrous magnesium sulfate, it was concentrated, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1) to obtain the title compound (146 mg, yield 90%). The compound was confirmed by identification of molecular weight using LC-MS. Calculated M=326.11, measured (M+H)+=327.2

1. extractionfollowed by extraction with ethyl acetate
2. dry with materialAfter drying the ethyl acetate phase with anhydrous magnesium sulfate, it
3. concentrationwas concentrated
4. customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1)