摘要
目的研究医药中间体N,N-二乙基乙醇胺（DEEA）的测定方法 ,以及DEEA在碱性介质中被二（过碘酸）合银（Ⅲ）配离子[Ag（HIO6）2]5-氧化的反应动力学和机理。方法采用紫外分光光度法。结果DEEA在（0.4～1.4）×10^-3mol/L内,其吸光度与浓度呈良好的线性关系,相关系数r=0.996,RSD为2.9%（n=6）。反应对Ag（Ⅲ）和DEEA均为一级,表观速率常数随[OH^-]的增大而增大,随[IO4^-]的增大而减小。结论该方法易掌握,成本低,结果准确,适于企业中间产品的质量控制。同时根据动力学实验结果提出了一个包括反应物与生成物形成的前期平衡在内的可能的反应机理,能很好地解释全部的实验现象。根据反应机理,导出了速率方程和速控步的速率常数值,计算出了活化参数。
Objective To explore the method to detect the concentration of N,N-Diethylethanol amine（DEEA） which currently being used as a Pharmaceutical Intermediates, and the kinetics of the oxidation of DEEA by bis （hydrogenperiodato） argentite （III） in an alkaline medium. Methods Spectrophotometry is applied in the experiment. Results The concentration of DEEA in the range of （0.4 ～1.4 ）×10 ^-3mol/L, plot of absorption against the concentration was linear, correlation coefficient r=0.996, RSD=2.9%（n=6）. The reaction was first order with respect to DEEA and Ag （III）, kobs increased with an increased of [OH^-], and decreased with an increased of [IO4^-]. Conclusion This method is easy to grasp, low cost and accurate, suitable for quality control of intermediate products in enterprise. A plausible mechanism of reaction involving a pre-equilibrium of adduct formation between complex and reductants was proposed, which could be applied to explain all experimental phenomena, and the activation parameers of the rate determining step have been also calculated.
出处
《医学研究与教育》
CAS
2010年第3期1-5,共5页
Medical Research and Education
基金
河北省自然科学基金资助课题(B2006000962)
关键词
N
N-二乙基乙醇胺
Ag(Ⅲ)
氧化
动力学与机理
紫外光谱
dimethylamino2-ethanol
Ag （III）
oxidation
kinetics and mechanism
ultraviolet spectropho-tometry
