摘要
以2-氧代戊二酸和水合肼为起始原料,经过环合、消除、酯化、三氯氧磷氯代4步反应合成6-氯哒嗪-3-甲酸甲酯,测定了中间产物的熔点,用^(1)H-NMR对目标产物结构进行表征。6-氯哒嗪-3-甲酸甲酯总收率80.1%(wt),液相纯度99.2%。此合成路线步骤少、容易操作、原料价格低、产物易于精制、收率高,适合放大生产6-氯哒嗪-3-甲酸甲酯。
The 6-chloropyridazine-3-carboxylicacid methyl ester is synthesized with the 2-oxoglutaric acid and hydrazine hydrate as raw materials through four steps which are cyclization,elimination,esterification and phosphorus oxychloride chlorination.The melting point of intermediate product is determined.The structure of target product is characterized with ^(1)H-NMR.The overall yield is 80.1%(wt),the purity of HPLC is 99.2%.This synthesis route has fewer steps,is easy to operate,has low raw material prices,is easy to refine the product,and has a high yield which make it suitable for scaling up the production of 6-chloropyridazine-3-carboxylicacid methyl ester.
作者
曹龙海
于振
王文彬
CAO Longhai;YU Zhen;WANG Wenbin(Institute of Petrochemistry,Heilongjiang Academy of Sciences,Harbin 150040,China)
出处
《化学与粘合》
CAS
2023年第6期508-510,共3页
Chemistry and Adhesion
基金
黑龙江省科学院石油化学研究院自拟课题(编号:2021-JSF-01)。
关键词
2-氧代戊二酸
6-氯哒嗪-3-甲酸甲酯
合成
2-oxoglutaric acid
6-chloropyridazine-3-carboxylicacid methyl ester
synthesis
