排序方式: 共有11条查询结果,搜索用时 109 毫秒
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以3-( 4-氟苯基) -1H-吡唑-5-甲酸乙酯为原料,与H2NNH2?H2O发生肼解生成3-( 4-氟苯基) -1H-吡唑-5-甲酰肼,再与CS2环化生成2-巯基噁二唑中间体,最后在巯基上进行烷基化反应合成了一系列新型的2-硫醚-5-吡唑基-1,3,4-噁二唑类化合物,并利用IR、1H NMR、HRMS等波谱技术对目标化合物结构进行了表征。该合成方法具有原料易得,后处理简便,收率较高的优点。 相似文献
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以3-吲哚甲酸与1-苯基-3-甲基-5-吡唑啉酮为原料合成3-甲基-1-苯基吡唑-5-基-1H-吲哚-3-甲酸酯(3),用IR、1 H NMR、热重分析、X-射线单晶衍射对化合物结构进行了表征,并对其荧光光谱进行了研究.X-射线单晶衍射结果表明:该晶体为斜方晶系,Pbca空间群,a=1.090 90(10)nm,b=1.618 93(14)nm,c=1.819 11(16)nm,α=β=γ=90.00°,V=3.212 7(5)nm3,Z=8,dC=1.312g/cm3,μ=0.088mm-1,F(000)=1 328. 相似文献
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The synthesis of 1,3,5-substituted-1,2,4-triazoles from α-imino-3-pyridine formic acid,acetamidine and anisole hydrazine as a model reaction in this paper and the synthesis mechanism of 1,3,5-substituted-1,2,4-triazole compounds from carboxylic acids,amidines and hydrazines have been first investigated with the B3 LYP/6-311++G** method.According to the potential energy profile,it can be predicted that the course of the reaction consists of five reactions containing six elementary reactions.The α-imino-3-pyridine formic acid and acetamidine form first an intermediate product through a dehydration reaction; the intermediate product further combines with hydrogen ion to form a positive ion; the positive ion reacts with anisole hydrazine by a dehydration reaction to form another positive ion; then,followed by two isomerization reactions,the final reaction with the acetate ion(Ac-) produces the final product.The research results reveal the laws of synthesis reaction of 1,3,5-substituted-1,2,4-triazoles by the carboxylic acids,amidines,hydrazines and their derivatives on theoretical level.It provides the systemic theoretical basis for the synthesis,development and application of 1,3,5-substituted-1,2,4-triazole compounds. 相似文献
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固相萃取-高效液相色谱电化学法检测大鼠血浆儿茶酚胺 总被引:2,自引:3,他引:2
建立了一种Oasis HLB固相萃取-高效液相色谱(HPLC)电化学检测大鼠血浆儿茶酚胺(CAs)的方法。血浆样本在形成二苯基硼酸-儿荼酚胺复合物后经优化的固相提取技术,得到较高样本回收率。以Atlantis C18色谱柱为固定相,确定了各种影响色谱的参数,如流动相组成、pH范围及检测器的设定。儿茶酚胺所有组分肾上腺素(E)、去甲肾上腺素(NE)和多巴胺(DA)的平均提取回收率在90%~95%之间。E、NE和DA的质量浓度在0.25~30ng/mL时与峰面积呈良好的线性关系(r值分别为0.9989,0.9992和0.9984);检出限为0.4pg。该法灵敏、准确、重现性好、结果可靠。 相似文献
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