摘要
2,4-二氯苯乙酮与甘油缩合,再经溴化、苯甲酰化、异构体分离、咪唑烷基化、水解和对甲苯磺酰化等过程得到了顺-2-(2,4-二氯苯基)-2-(1H-咪唑基-1-甲基)-1,3-二氧戊环-4-甲基对甲苯磺酸酯。对现行工艺主要进行了三点改进:缩合反应中以正戊醇代替正丁醇作为带水剂;咪唑烷基化反应中以甲苯代替DMF溶剂,以KI代替NaCN作为催化剂;对甲苯磺酰化反应中以三乙胺代替吡啶作为缚酸剂,总收率提高为27.6%。目标产物经1H NMR和IR表征。
cis-[2-（2,4-Dicholoro-phenyl）-2-（1H-imidazole-l-ylmethyl）-l,3-dioxolane-4-yl] methyl p-toluenesulfonate was synthesized from 2,4-dichloroacetophenone through glycerol cyclization, bromi- nation, benzoylation, isomeric separation, N-alkylation, hydrolysis and tosylation. Three improvements of this process were that n-amyl alcohol was substituted for normal butanol in glycerol eyelization, toluene and KI were substituted respectively for DMF and NaCN in the N-alkylation, pyridine was re- placed by triethylamine as acid-binding agent in tosylation, and the total yield is 27.6%. The aimed re- sult was characterized by 1HNMR and IR.
出处
《江苏技术师范学院学报》
2013年第2期12-15,共4页
Journal of Jiangsu Teachers University of Technology
关键词
2
4-二氯苯乙酮
酮康唑活性酯
工艺改进
2,4-dichloroacetophenone
ketoconazole activity ester
process improvement
