1,2-Dichloroethane → HCID 131727863, compound

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Reaction Steps

Next, 62.5 g of the 4,6-di(1-adamantyl)-1,3-bis(4-carboxy-phenoxy)benzene dipotassium salt obtained above (90 mmol), 200 mL of 1,2-dichloroethane and a stirrer were charged in a 2 L recovery flask. Then, 178.5 g of thionyl chloride mol) was gradually added thereto with agitating at 5° C. or less. After the addition, 1.5 mL of N,N-dimethylformamide and 1.5 g of hydroquinone were added and agitated at 45 to 50° C. for three hours. After reaction solution was filtered, solvent was removed from the reaction solution under reduced pressure. Solid thus obtained was washed with hexane and then recrystallized with diethyl ether, thus obtaining 38.9 g of 4,6-di(1-adamantyl)-1,3-bis(4-carboxy-phenoxy)benzene-dichloride (59.4 mmol; yield: 66.0%).

Provenance & Evidence