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在优良抗风湿药物萘普生的重要中间体6-甲氧基-2-乙酰素的合成中存在溶剂硝基苯的毒性及所带来的污染。而改用二氯乙烷作溶剂,只加少量硝基苯即可。为配合合成工艺的优化,用气相色谱(GC)、气相色谱-质谱(GC/MS)对反应产物、副产物及多个杂质进行了定性分析研究,并在5%OV-101ChromosorbWAWDMCS柱上完成了产物的内标定量分析。从而减少了副反应和高沸点杂质的生成,最终生产出了95%以上含量的6-甲氧基-2-乙酰萘产品,收率达到60%。
In the synthesis of 6-methoxy-2-acetoxyproline, an important intermediate of naproxen, an excellent anti-rheumatic drug, there is toxicity and pollution caused by nitrobenzene. Instead of using dichloroethane as a solvent, only a small amount of nitrobenzene can be added. In order to optimize the synthesis process, the reaction products, by-products and many impurities were qualitatively analyzed by gas chromatography (GC) and gas chromatography-mass spectrometry (GC / MS), and the results were obtained on a 5% OV-101 Chromosorb WAWDMCS column Internal standard quantitation of the product. Thereby reducing side reactions and the formation of high-boiling impurities, finally producing more than 95% of the 6-methoxy-2-acetyl naphthalene product yield of 60%.