固—液相转移催化N-烷基化反应——Azone的合成

SOLID-LIQUID PHASE TRANSFER CATALYTIC N-ALKYLATION—SYNTHESIS OF AZONE

Azone(1—十二烷基氯杂环庚烷—2—酮)是一种新型高效透皮吸收促进剂。采用固—液相转移催化法,由己内酰胺与氯代十二烷,在相转移催化荆聚乙二醇和固体氢氧化钾存在下,于112℃回流8小时制得。相转移催化剂以PEG 400为好,PEG/KOH为0.88(重量比),己内酰胺:氯代十二烷:KOH为1.1∶1∶2.95(摩尔比),产率可达84.6％～89.4％。

Azone (1-dodecylazacyclo heptan-2-one) is a novel penetration enhancer. This paper describes the prepapration of Azone from 1-chloro dodecane and caprolactam in powder KOH-PEG system by a solid-liquid phase transfer catalysis process. The optimum conditions are PEG400, PEG/KOH=0.88(by wt.) caprolactam: 1-chlorododecane: KOH=1.1: 1: 2.95(by mol.), reaction temperature 112℃, reaction time 8 hours. Yield ranges from 84.6% to 89.4%.