A simple, effective and reliable synthetic method was developed to construct beta-agonist phenylethanolamine A(PEAA) in good yield with 4-nitrobenzyl bromide as the starting material, which underwent SN2 reaction with ethyl acetoacetate, followed by hydrolysis with concentrated HCl and amination by Leukart reaction to furnish 4-(4-nitrophenyl)butan-2-amine(A). A one-pot reaction was studied to construct PEAA skeleton and reduced carbonyl with KBH4, the conditions were optimized, including reaction temperature, reaction time, solvent and the molar ratio of 2-bromo-1-(4-methoxyphenyl)ethanone(B) to A. Meanwhile, a reliable and practical high performance liquid chromography(HPLC) method with UV detector was developed after screening wavelength, chromatographic column and optimization of mobile phase. The optimal conditions of detecting PEAA were water(0.1% formic acid and 0.1% triethylamine)-methanol(volume ratio 44:56) at 278 nm with plus-C18 column. The above synthetic method would be used to synthesize standard reference materials and advance extensive application of analytical method. In order to ensure food safety and safeguard human health, the analytical method might be used as a standard method in detection and supervision of PEAA.

中文翻译：

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苯乙醇胺A的全合成及高效液相色谱分析

开发了一种简单，有效，可靠的合成方法，以4-硝基苄基溴为起始原料，高收率构建β-激动剂苯基乙醇胺A（PEAA），使其与乙酰乙酸乙酯进行SN2反应，然后用浓HCl水解，并经胺化处理。通过Leukart反应得到4-（4-硝基苯基）丁-2-胺（A）。研究了用一锅法构建PEAA骨架并用KBH4还原羰基的条件，优化了反应温度，反应时间，溶剂和2-溴-1-（4-甲氧基苯基）乙酮（B）的摩尔比等条件。同时，通过筛选波长，色谱柱和优化流动相，开发了一种可靠且实用的带有紫外检测器的高效液相色谱法。用plus-C18色谱柱检测PEAA的最佳条件是在278 nm处水（0.1％甲酸和0.1％三乙胺）-甲醇（体积比44:56）。上述合成方法将用于合成标准参考物质，并促进分析方法的广泛应用。为了确保食品安全和维护人体健康，该分析方法可以作为检测和监督PEAA的标准方法。