摘要
α-卤代腙与α-异氰酸酯在三乙胺作用下反应,生成4-腙基-2-异氰基丁酸酯类化合物。通过优化合成工艺,确定最佳反应条件为:α-卤代腙(1.0 eq.),α-异氰酸酯(1.2 eq.),三乙胺(1.2 eq.),二氯甲烷作溶剂,反应24 h。在此条件下进行了底物普适性研究,以高达79%的收率得到一系列具有潜在价值的4-腙基-2-异氰基丁酸酯类化合物,产物结构经1H NMR,13C NMR和MS(ESI)确证。
A series of 4-hydrazineylidene-2-isocyanobutanoates with potential values were obtained in up to 79%yield by the reactions ofα-isocyano esters withα-halo hydrazones.The optimal conditions were confirmed:α-halo hydrazones(1.0 eq.)andα-isocyano esters(1.2 eq.)in CH2Cl2 with Et3N(1.2 eq.)at room temperature for 24 h.The structures were confirmed by 1H NMR,13C NMR and MS(ESI).
作者
全保学
赵建强
袁伟成
QUAN Bao-xue;ZHAO Jian-qiang;YUAN Wei-cheng(Chengdu Institute of Organic Chemistry, Chinese Academy of Sciences, Chengdu 610041, China;Institute for Advanced Study, Chengdu University, Chengdu 610106, China;University of Chinese Academy of Sciences, Beijing 100049, China)
出处
《合成化学》
CAS
北大核心
2020年第10期890-895,共6页
Chinese Journal of Synthetic Chemistry
基金
国家自然科学基金资助项目(21871252,21901024)。
关键词
α-异氰酸酯
α-卤代腙
三乙胺
工艺优化
合成
α-isocyano ester
α-halo hydrazone
triethylamine
process improvement
synthesis