Hydrochloric Acid → HCID 66776473, compound

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Reaction Steps

In a 300 mL three-neck flask, 410 mg (17 mmol) of active magnesium was stirred in 5 mL of dehydrated tetrahydrofuran (THF), and about 0.2 mL of 1,2-dibromoethane was added thereto, so that bubble release and heat generation were confirmed. A solution in which 5.2 g (15 mmol) of 4-bromophenyl-1-phenyl-1H-benzimidazole has been dissolved in 50 mL of dehydrated THF was added thereto. The mixture was heated and stirred for 4 hours, and then cooled to room temperature, so that a Grignard reagent was prepared. Then, in a 500 mL three-neck flask were put 3.7 g (17 mmol) of 4-bromobenzoyl chloride and 150 mL of dehydrated THF, and the mixture was stirred at −40° C. The above Grignard reagent was dropped into the mixture, the mixture was stirred for 1 hour, and then stirred at room temperature for about 15 hours. After reaction, 1N-hydrochloric acid was added to the mixture until the mixed solution became acid. An organic phase of the obtained mixed solution was washed with water, and then magnesium sulfate was added thereto so that moisture was adsorbed. This suspension was filtered, the resulting filtrate was concentrated, and ethyl acetate and toluene were added to perform recrystallization. As a result, 2.5 g of powder was obtained. The reaction scheme is shown in (A-1).

Provenance & Evidence