第 50 卷第 5 期Vol. 50 No. 5
2020 年 10 月Oct 2020

所属栏目:医药及中间体

脱氢枞基酰基吡唑化合物的合成与表征
伍 勇,黄春花,徐 静 (四川卫生康复职业学院 药学系,四川 自贡 643000)
摘 要:以脱氢枞酸为原料,在二氯甲烷溶剂中与二氯亚砜酰化合成脱氢枞酰氯(2);无水碳酸钠作缚酸剂,脱氢枞酰氯(2)与80%水合肼在四氢呋喃溶剂中,常温条件下生成脱氢枞酰肼(3);脱氢枞酰肼(3)与乙酰丙酮经三乙胺催化,在N,N-二甲基甲酰胺溶剂中回流8 h,最终脱水成环生成脱氢枞基酰基吡唑化合物(1),收率43.3%。产物结构经核磁共振氢谱、碳谱及红外光谱确证。
关键词:脱氢枞酸;吡唑;合成
中图分类号:TQ252.1  文献标识码:A  文章编号:1009-9212(2020)05-0021-03
Synthesis and Characterization of Dehydroabietyl Pyrazole Compound
WU Yong, HUANG Chun-hua, XU Jing (Department of Pharmacy, Sichuan Vocational College of Health and Rehabilitation, Zigong 643000, China)
Abstract:Using dehydroabietic acid as raw material, dehydroabietic acid chloride (1) was synthesized in methylene chloride solvent with thionyl chloride; and then, anhydrous sodium carbonate as acid binding agent, dehydroabietic hydrazide (2) was prepared from product 1and 80% hydrazine hydrate in tetrahydrofuran solvent normal temperature conditions; the last, dehydroabietyl pyrazole compound(3), in yield of 43.3%, was obtained from product 2 and acetylacetone, which were catalyzed by triethylamine and were refluxed in N,N-dimethylformamide solvent for 8 hours; the product structure was characterized by IR, 1H NMR and 13C NMR.
Key words:dehydroabietic acid; pyrazole; synthesis
基金项目:自贡市重点科技计划资助项目(2018CZ30),四川卫生康复职业学院重点项目(CWKY-2018Z-03)。
作者简介:伍 勇(1975—),男,四川荣县人,副教授,硕士,主要从事天然产物化学研究(E-mail:wuyongrx@163.com)。
收稿日期: 2020-10-1