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利奈唑酮是新上市的一种口恶唑烷酮类全合成抗菌药,本研究对其关键中间体(R)-N-[[3-[3-氟-4-吗啉基]苯基]-2-氧代-5口-恶唑烷基]甲醇(1)的合成方法做了改进.合成3-氟-4-吗啉基硝基苯时,用价廉易得的三乙胺代替二异丙基乙胺,反应时间由72h缩短到6h;合成3-氟-4-吗啉基苯胺时,将溶媒改为丙酮,采用Pd/C(10%)还原,反应液直接与氯甲酸苄酯反应制得N-苄氧羰基-3-氟-4-吗啉基苯胺,实现了两步合一,收率提高到93.2%;合成(1)时,反应温度提高到-50℃左右,实验条件较文献方法相对温和.
Linezolidone is a newly marketed oxazolidinone synthetic antibacterial agent. In this study, its key intermediates (R) -N - [[3- [3-fluoro-4-morpholinyl] phenyl ] -2-oxo-5-oxazolidinyl] methanol (1) was synthesized in the synthesis of 3-fluoro-4-morpholino nitrobenzene, with cheap and readily available triethylamine Instead of diisopropylethylamine, the reaction time was shortened from 72h to 6h; when the 3-fluoro-4-morpholinoaniline was synthesized, the solvent was changed to acetone and reduced with Pd / C (10% Benzyloxycarbonyl-3-fluoro-4-morpholinoaniline was obtained by the reaction of benzyl formate, and the yield was increased to 93.2%. The synthesis of (1), the reaction temperature was increased to -50 ℃ , The experimental conditions are relatively mild compared with the literature method.