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出 处:《质谱学报》2011年第6期367-373,共7页Journal of Chinese Mass Spectrometry Society
摘 要:以高效液相色谱-串联质谱的形式建立一种简单、快速的正交反应优化手段。在优化的条件下合成了两个脯氨酸有机催化剂。该方法不仅能找到最佳的反应条件,还能确定各因素之间对反应作用的强弱,同时还能在不影响产物稳定性的情况下,依靠高效液相色谱的高效分离功能对原料和产物进行分离;通过质谱的强定性能力监控反应,并对无生色基团的产物进行鉴定,从而对反应机理做进一步解释。该方法明确了脯氨酸有机催化剂的最佳合成条件,快速、准确地鉴定了产物及其纯度,是一种省时、经济、有效的研究方法和分析手段,可以用于有机反应监控和产物分析。A simple and efficient synthesis optimization method for two proline organocatalysts based on the application of LC-MS/MS was reported. We not only found the best synthetic conditions for proline organocatalysts, but also figured out the different effects of each individual factor. The synthetic products could be well isolated from the reagents based on the optimized HPLC method. At the same time, by taking advantage of the strong structure illustration ability of tandem mass spectrometry, we were able to identify the mo- lecular structure of the proline organocatalysts and further understand the related synthetic mechanisms. The method we established found the best synthetic conditions for proline or- ganocatalysts and identified the products and their purities rapidly and accurately. It was a time-saving, economical and effective research method and analytical tool, which could be used for monitoring organic reactions and identifying their products.
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