阿克他利的合成

以苯乙腈为原料,经硝化、水解、还原以及酰化等4步反应对阿克他利(Actarit,对乙酰氨基苯乙酸)及其中间体的合成条件进行了研究和改进.目的产物用元素分析、红外光谱及核磁共振氢谱进行了表征.研究发现对硝基苯乙腈合成的最适温度为7~8℃.在回流温度152℃,对硝基苯乙腈水解且搅拌充分的情况下效果最为理想,对硝基苯乙酸的还原以水溶液中醋酸活化的铁粉为还原剂效果较好.乙酸酐与对氨基苯乙酸的比例为1.5∶1(物质的量比)时对乙酰氨基苯乙酸的合成较好,4步反应总收率可达50.5%.

Study on the Synthesis of Actarit

The title compound was prepared from phenylacetonitrile by nitration,hydrolysis,reduction,and acylation.The structure was determined by elemental analysis,IR and 1H NMR spectra.The optimal conditions were indicated as follows: the appropriate temperature for the preparation of 4-nitrobenzyl cyanide was 7～8 ℃,the optimal temperature for hydrolysis of 4-nitrobenzyl cyanide was 152 ℃,4-nitrophenylacetic acid was reduced in water with Fe powder which was activated by acetic acid and the optimal ratio of acetic anhydride to 4-aminophenylacetic acid was 1.5∶1.The overall yield reached 50.5 % under the above conditions.