5-甲基-4-异噁唑甲酰肼的合成研究

Synthesis of 5-Methyl-4-Isoxazole Formyl Hydrazine

以乙酰乙酸乙酯为起始原料,经缩合、环合、水解得到5-甲基-4-异噁唑甲酸,再与氯化亚砜、水合肼反应得5-甲基-4-异噁唑甲酰肼(三氮唑类衍生物重要中间体),并研究了温度、原料配比和加料顺序等对合成的影响。化合物6结构经IR、1H-NMR、13C-NMR、MS等确证正确。该方法原料易得、操作简便,后两步收率为65%,产品纯度达到98%。

5-methyl-4-isoxazole-formyl hgdrazine, a key intermediate of triazole derivatives, was synthesized via 5 steps. 5 -methyl-4-isoxazoleearboxylie acid chloride was obtained from ethyl aeetoaeetate by condensation, eyelization and hgdrolyzation and chlorination, which was reacted with hgdrazine to give the desired product in an overall yield of 33%. Whereas the influence of the reaction temperature, the materials proportion and the mode of adding materials on synthesis was studied. The structure of compound 6 was eomfirmed by IR, ^1 H-NMR, ^13C-NMR, MS, etc. The improved sythetie route featured accessible starting materials and easy performance.