摘要
目的:1、用d-伪麻黄碱(Pseoduphedine)做拆分剂拆分扁桃酸,建立适合于工业化生产的拆分工艺。2、回收伪麻黄碱,解决拆分剂昂贵问题,3、提供新的拆分剂:光学纯扁桃酸。方法:1、将拆分剂d-伪麻黄碱与dl-扁桃酸混合,在无水乙醇中成盐,加入含Ca2+溶液,析出沉淀,分别对沉淀和母液进行处理,得到d-扁桃酸和l-扁桃酸粗品,用甲苯重结晶,获得光学纯d-扁桃酸和l-扁桃酸。2、将反应中形成的盐酸伪麻黄碱溶液,用NaOH调至碱性,析出伪麻黄碱,用乙醇重结晶,回收可重复使用的d-伪麻黄碱。结果:1、获得d-扁桃酸,收率为74.7%,光学纯度(ee%)98.7%、l-扁桃酸收率为91.1%,光学纯度(ee%)68.4%、总收率为82.9%。2、伪麻黄碱回收率为85.5%,%ee大于98%。结论:1、解决了伪麻黄碱拆分扁桃酸的技术难点,Ca2+离子促进d-伪麻黄碱·d-扁桃酸盐沉淀;2、工艺条件满足拆分要求:3、成功回收伪麻黄碱,解决拆分剂昂贵问题,4、获得新的拆分剂:d-扁桃酸;5、为伪麻黄碱在化学领域找到了作拆分剂的应用。
Objective:1 To resolve racemic mandelic acid With d-Pseudoephedrine as resolution agent and establish the technological process to suit the industrial production . 2 To recover d-pseudoephedrine so that made utilization of resolution agent. 3 To provide a new resolution agent of: optically pure mandelic acid. Methods: 1 Mixed d-pseudoephedrine and dl-mandelic acid in unhydrated alcohol ,add saturated Ca2+ solution, separate the precipitate and liquor ,get the d-and l-mandelic acid. 2 Adjusted the pseudoephedrine hydrochloride solution with NaOH to alkalinity,get the pseudoephedrine. Results: 1 For The d-mandelic acid,general yield is 91.1%,the optical purity(%ee) is 98.7%; for the l-mandelic acid,the optical purity is 85.1% and general yield is 91.1%。2 The recycle rate of pseudoephedrine is 85.5%. Conclusion: 1 Resolve the technical difficulties of pseudoephedrine as the resolution reagent to separate racemic mandelic acid; 2 The technological process conform to the request of resolution and broaden the scope of the application of pseudoephedrine. 3 Recycling the Pseudoephedrine is successful,utilization of Pseudoephedrine as resolution agent further;4 Get a new resolution agent: optically pure mandelic acid; 5 Find a new application in the chemical field of pseudoephedrine .
引文
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