CAJ | 학술논문

为进一步探讨双酰肼羧酸酯的合成方法，以水杨酸甲酯和水合肼为原料，首先合成了水杨酰肼，再与顺丁烯二酸酐反应，合成了（Z）-3-水杨酰肼羰基丙烯酸（（Z）-H4shcpa）。然后由（Z）-H4shcpa和FeCl3·6H2O进一步构造了金属冠醚体系。通过内部自催化反应，（ Z）-H4 shcpa发生酯化，经过SnCl2/HCl溶液还原体系处理，最终得到了乙酯化的产物（Z）-3-水杨酰肼羰基丙烯酸乙酯（（Z）-H3eshcp）。对目标化合物进行了IR、1H-NMR、13C-NMR和元素分析等表征，结果表明：通过内部自催化反应，经由金属冠醚体系，可以解决双酰肼羧酸乙酯的合成难题。
위진일보탐토쌍선정최산지적합성방법，이수양산갑지화수합정위원료，수선합성료수양선정，재여순정희이산항반응，합성료（Z）-3-수양선정탄기병희산（（Z）-H4shcpa）。연후유（Z）-H4shcpa화FeCl3·6H2O진일보구조료금속관미체계。통과내부자최화반응，（ Z）-H4 shcpa발생지화，경과SnCl2/HCl용액환원체계처리，최종득도료을지화적산물（Z）-3-수양선정탄기병희산을지（（Z）-H3eshcp）。대목표화합물진행료IR、1H-NMR、13C-NMR화원소분석등표정，결과표명：통과내부자최화반응，경유금속관미체계，가이해결쌍선정최산을지적합성난제。
To obtain a synthesis method of the esterification of carboxylic acid with bis-hydrazide, salicylhydrazide was prepared using methyl salicylate and hydrazine hydrate , followed by reaction with maleic anhydride to produce ( Z )-3-( salicylhydrazinocarbonyl ) propenoic acid ( ( Z )-H4 shcpa ) .A metallacrown system was then formed by reaction with FeCl3· 6H2O.The ligand was esterified and transformed into (Z)-ethyl 3-(salicylhydrazinocarbonyl) propenoate ((Z)-H3 eshcp) through internal self-catalytic reaction.The metallacrown can be treated with SnCl 2/HCl to obtain purified ester ( Z)-H3 eshcp in good yield .The structure of these compounds were characterized by IR , 1 H-NMR, 13 C-NMR and element analysis.It showed that the difficult problem of ethyl-esterification of carboxylic acid with bis-hydrazide can be solved through the internal self-catalytic reaction of metallacrown system .