Lu Xiao-qin
2010
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Journal
Fine chemicals
Abstract
4-[(4-Methylpiperazin-1-yl)methyl]benzoic acid dihydrochloride was synthesized from 4-methylbenzoic acid via the α-bromination and acidification after amination without separation.The effects of the bromine agent and initiator on the bromination,and that of material ratio,temperature and time on amination were investigated.The optimized conditions were:bromosuccinimide as bromine agent,benzoyl peroxide as the initiator,the yield of 4-(bromomethyl)benzoic acid was close to 88.7%;the ratio of 4-(bromomethyl)benzoic acid to 1-methylpiperazine 1∶1.2,sodium bicarbonate as the acid binding agent,the reaction temperature ranges from 20~25 ℃,the reaction time 8 h.The yield of product under these optimum reaction conditions was up to 81.5%.The structure of the product was confirmed by melting point,IR and 1HNMR.