67085-11-4

288-32-4

59363-13-2

67085-11-4

(2) In a dry DMF solvent, sodium hydride (in the form of mineral oil dispersion) at a concentration of 20% was added and 20 mL of a DMF solution of imidazole was added dropwise at a rate of 2 mL/s under ice bath cooling conditions. Subsequently, the reaction mixture was stirred at 60 °C for 60 min. After the ice bath was cooled, Intermediate 1 (weight ratio of imidazole, sodium hydride to Intermediate 1 was 7:7:5) was slowly added via the salt bath method. The reaction mixture was continued to be stirred at 60°C for 120 minutes. After completion of the reaction, the reaction was again cooled in an ice bath and a 25% n-hexane solution was added to the reaction mixture and stirred at a rate of 3 rev/s for 15 min. Subsequently, ice (350% by weight of the reaction mixture) was added and stirring was continued at a rate of 3 rev/s until the precipitation was complete. The precipitate was collected by filtration and the filter cake was washed once with water and then dried by centrifugation at 2830 r/min for 60 minutes. The resulting product was treated with 2.5 times its weight of ethyl acetate and 0.05 times its weight of activated charcoal, left to stand at 5 °C for 13 h, followed by recrystallization at 50 °C. The yield of Intermediate 2 was 71.5% by HPLC analysis, wherein the purity of the target product 1-[4-(4-chlorophenyl)-2-hydroxy-n-butyl]imidazole was 99.31%.