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  • 左乙拉西坦的合成_制药工程论文范文

    制药工程论文范文 目 录 中文摘要I 英文摘要II 目录III 1. 绪论1 1.1 癫痫简介1 1.2抗癫痫药研究进展1 1.3抗癫痈药物分类3 1.4 左乙拉西坦概况4 1.4.1药效特点4 1.4.2上市情况5 1.4.3市场预测5 1.4.4左乙拉西坦的未来预测5 1.5 左乙拉西坦合成路线选择6 1.5.1左乙拉西坦反合成分析6 1.5.2左乙拉西坦合成路线分析7 1.6左乙拉西坦的合成 ----以2-溴丁酸为起始原料进行合成11 2. 实验部分13 2.1制备2-氨基丁酸 13 2.2制备2-氨基丁酸甲酯13 2.3制备氨基丁酰胺14 2.4制(S)-氨基丁酰胺。酒石酸15 2.5制备(S)-氨基丁酰胺盐酸盐15 2.6 由R-(-)-2-氨基丁酰胺转变为消旋的(RS)型:15 2.7 制备左乙拉西坦:15 2.8 左乙拉西坦的精制:16 3. 结果与讨论17 3.1制备2-氨基丁酸 17 3.2制备2-氨基丁酸甲酯————酯化反应18 3.3 制备2-氨基丁酰胺 19 3.4制备(S)-2-氨基丁酰胺酒石酸————拆分 20 3.5制备(S)-氨基丁酰胺。盐酸盐 20 3.6由(R)-2氨基丁酰胺转变成混旋的2-氨基丁酰胺——消旋反应R型和S型 之间转变 21 3.7 制备(S)-2-乙基-2-氧-1-吡咯烷乙酰胺(左乙拉西坦)-关环22 3.8 左乙拉西坦的精制 24 3.9 实验最后结果25 致谢26 参考文献27 摘要: 本论文在已有文献的基础上,简要地叙述了抗癫痫药物治疗的研究进展,重点阐述了抗癫痫药(S)-2-乙基-2-氧-1-吡咯烷乙酰胺的合成工艺。筛选以2-溴代丁酸为起始原料,经氨解,酯化,酯胺解,拆分,环合五步反应制得左乙拉西坦。所用酯化方法采用HCL/甲醇和二氯亚砜和硫酸分别进行实验研究,胺解分别采用饱和甲醇胺,加无机盐,加水三种方案进行实验。拆分采用非对映异构体拆分方法,在有机溶剂中用酒石酸为拆分剂,得到S型。同时本论文也对拆分后的R型异构体进行转变消旋而重回收。另外本实验直接采用(S)-(+)-2-氨基丁酰胺酒石酸盐进行关环实验,跳过了先制备(S)-(+)-2-氨基丁酰胺盐酸盐,再关环制备左乙拉西坦的一步。本合成路线总收率为25%。本工艺路线操作简便,成本低,收率高,可进行工业化大规模生产。 关键词:左乙拉西坦; 合成 ; 抗癫痫药物 Abstract: In this paper, the existing literature on the basis of a brief description of the antiepileptic drug therapy, with a focus on antiepileptic drug (S) -2 - ethyl -2 - O -1 - pyrrolidine acetamide Technology. Screening for 2 - bromo-butyric acid as the starting material, after ammonolysis, esterification, ester amine solution, split, five-step cyclization reaction Levetiracetam. Methods used in esterification HCL / methanol and dichloro-sulfoxide and sulfuric acid to carry out experimental research aminate methanol saturated amines were used, plus salt, add water, three options to conduct experiments. Resolution of the use of non-resolution of enantiomers methods used in organic solvents tartaric acid for the separation agent, to be S-type. At the same time, this paper also split the R-isomer of racemic to change and re-recovery. Another direct use of this experiment (S )-(+)- 2 - tartaric acid amide ammonium salt hybroxybutyric cyclization experiments skip the first preparation of (S )-(+)- 2 - ammonia hybroxybutyric amide hydrochloride, and then related Preparation of Levetiracetam ring step. The synthetic route for the 25% overall yield. The process line is simple, low cost, high yield, large-scale production can be industrialized. Keywords: Synthesis; Levetiracetam ; Antiepileptic drug

  • (R)-2-羟基-4-苯基丁酸乙酯的合成_制药工程论文

    制药工程论文范文 目 录 中文摘要...................................................................Ⅰ 英文摘要...................................................................Ⅱ 目录.......................................................................Ⅲ 1.绪论......................................................................1 1.1 前言................................................................1 1.2 概述................................................................2 1.2.1拆分法.........................................................2 1.2.2合成法.........................................................3 1.3 本章小结............................................................4 2.实验部分..................................................................6 2.1 实验仪器与试剂......................................................7 2.1.1实验仪器.....................................................7 2.2.2分析检测仪器.................................................7 2.1.3实验试剂.....................................................7 2.2 反应路线............................................................7 2.3 2,4-二氧代苯基丁酸乙酯的合成........................................7 2.4 (R)-2-羟基4-氧代苯基丁酸乙酯的合成..................................8 2.5 (R)-2-羟基4-苯基丁酸乙酯的合成......................................8 2.6 本章小结............................................................8 3.结果与讨论................................................................9 3.1 对合成2,4-二氧代苯基丁酸乙酯的各因素的探讨..........................9 3.1.1不同催化剂对收率的影响........................................9 3.1.2不同反应物摩尔比对收率的影响..................................10 3.1.3不同反应温度对收率的影响......................................11 3.1.4不同反应溶剂对收率的影响......................................11 3.2 对合成(R)-2-羟基-4-氧代苯基丁酸乙酯的反应条件的探讨................13 3.2.1收率与e.e%的两者关系探讨.....................................13 3.2.2修饰剂用量对不对称加氢的影响.................................14 3.3 合成(R)-2-羟基-4-苯基丁酸乙酯的收率及表征..........................14 3.4 本章小结...........................................................15 4.总结与展望..............................................................16 致谢.......................................................................17 参考文献...................................................................18 摘 要:(R)-2-羟基-4-苯基丁酸乙酯是合成众多血管紧张素转化酶抑制剂(ACEI)类治疗高血压和充血性心力衰竭药物的关键手性中间体。本文阐述了以苯乙酮、草酸二乙酯为原料最终合成(R)-2-羟基-4-苯基丁酸乙酯的合成路线。并对合成2,4-二氧代苯基丁酸乙酯的反应条件作了优化探讨,最终发现当以甲苯为溶剂,乙醇钠为催化剂,反应温度为30℃,反应时间为2小时,转化率可达到39.1%。而且对本实验中的Raney Ni催化加氢步骤也作了研究;修饰剂的用量,反应时间,氢气压力对于合成对映体的量有很大的影响。最终发现,当修饰剂用量为7mg,反应时间为150min,其转化率、不对称选择效果可达到最大值。不对称选择性效果并不随着反应时间的增加而增大,反而会随着反应时间的增大而减小。本文为工业化生产制备该类药物提供了一些可行的方法和途径。 关键字:加氢; (R)-2-羟基-4-苯基丁酸乙酯;修饰剂; Abstract: A synthesis route to produce ethyl (R)-2-hydroxy-4-phenylbutyrate, an important intermediate for several ACE inhibitors is described starting from acetophenone and diethyl oxalate. Ethyl 2,4-dioxo-phenylbutyrate is synthesized from acetophenone and diethyl oxalate by using different conditions,the optimal condition is founded. The reaction was run in aqueous toluene at 30℃ for 2h under the catalysis of Sodium ethoxide. The yield is 39.1%. Also the condition of the hydrogenation of ethyl 2,4-dioxo-4-phenylbutyrate catalyzed by a heterogeneous Raney Ni catalyst is studied . The effects of modifier amount, reaction time, hydrogen pressure and temperature on enantiometric excess are investigated to synthesize ethyl (R)-2-hydroxy-4- phenylbutyrate. It is found that conversation and enantioselectivity showed a maximum in the condition of modifier amount is 7mg for 150min. The conversation increased with the increase of reaction time,which almost had no effect on the enantioselectivity, but it had adverse influence on enantiomeric excess. The study provides a practicable method for industrial production of this remedy. Keywords: Hydrogenolysis; Ethyl (R)-2-hydroxy-4-phenylbutyrate; Modifier;

  • 红色素的制备及性质的研究_制药工程论文范文

    制药工程论文范文 目 录 中文摘要Ⅰ 英文摘要Ⅱ 目录Ⅲ 1. 绪论1 1.1 红曲2 1.2 红曲霉3 1.3 红色素的组成及生成机制3 1.3.1 红色素的组成.............................................3 1.3.2 红色素的生成机制.........................................3 1.4 红色素的一般性质……………………………………………………………4 1.5 红色素的生产方法……………………………………………………………4 1.5.1厚层通风制曲工艺………………………………………………………4 1.5.2 液体发酵生产红曲色素…………………………………………………5 1.6 红色素的应用…………………………………………………………………5 1.6.1在肉制品的应用 …………………………………………………………5 1.6.2在腌菜蔬菜中的应用 ……………………………………………………5 1.6.3在面包生产中的应用 ……………………………………………………5 2 实验部分 ………………………………………………………………………………6 2.1 材料 ……………………………………………………………………………6 2.1.1 菌种 ………………………………………………………………………6 2. 1.2 培养基 ……………………………………………………………………6 2.1.3 仪器与设备 ………………………………………………………………6 2.1.4 试剂 ………………………………………………………………………6 2.2 实验方法…………………………………………………………………………6 2.2.1 菌种活化……………………………………………………………………6 2.2.2 菌种分离纯化………………………………………………………………7 2.2.3 孢子悬浮液的制备…………………………………………………………7 2.2.4 初筛……………………………………………………………………………7 2.2.5 复筛……………………………………………………………………………7 2.2.6 传代稳定性实验………………………………………………………………7 2.3 菌体形态观察方法…………………………………………………………………7 2.4 红色素色价测定方法………………………………………………………………8 2.5 红色素稳定性研究…………………………………………………………………8 2.5.1 色素的光谱特性………………………………………………………………8 2.5.2温度对红色素稳定性的影响…………………………………………………8 2.5.3 pH值对红色素稳定性的影响 ………………………………………………8 2.5.4 光对红色素的稳定性的影响 ………………………………………………8 2.5.5 氧化剂和还原剂对红色素稳定性的影响…………………………………9 2.5.6 防腐剂对红色素稳定性的影响 ……………………………………………9 2.6 色素提取……………………………………………………………………………9 3 结果与分析…………………………………………………………………………………10 3.1分离纯化结果与分析………………………………………………………………10 3.2 红色素稳定性实验分析…………………………………………………………12 3.2.1红色素光谱特性的研究………………………………………………………12 3.2.2 温度对红色素稳定性影响的研究……………………………………………13 3.2.3 pH值对红色素稳定性影响的研究…………………………………………14 3.2.4 光照对红色素稳定性影响的研究 …………………………………………14 3.2.5 氧化还原剂对红色素稳定性影响的研究 …………………………………15 3.2.6 防腐剂对红色素稳定性的影响 ……………………………………………15 4 总结与展望 ………………………………………………………………………………17 4.1 总结…………………………………………………………………………………17 4.2 展望…………………………………………………………………………………17 致谢 …………………………………………………………………………………………18 参考文献 ……………………………………………………………………………………19 摘 要:本课题以产色素真菌为材料,通过菌株的筛选得到高产色素菌株, 并对其各项理化性质及其色素提取工艺进行研究;运用液态发酵法生产红色素,并对红曲霉的培养基条件进行优化。确定红色素的最大吸收峰在505nm处,红曲霉最佳发酵天数为6~7天,适宜的培养基配方为: 大米粉9 % , NaNO3 0. 2 % , KH2 PO4 0.1 % , MgSO4 0. 2 %。在红色素的稳定性研究中发现,红色素在常温条件下是比较稳定的,pH值在5~7之间对红色素稳定性的影响是比较微弱的,偏于极端的pH值对红色素稳定性的影响是比较大的。室内室外光照对红色素稳定性影响均不大。红色素稳定性不受常见金属离子的影响。防腐剂对红色素的影响不明显,并且不受浓度的影响。 关键词:红曲霉;红色素;稳定性;提取 Abstract:The fungus is subject to production of the pigment material,,through high-yield strains of pigmented strains screened,,and their various physical and chemical properties of pigment extraction technology research to the further development of the fungal pigment provide the scientific basis。 This paper describes the chemical composition of red pigment and its general nature,by liquid fermentation of Monascus red pigment production media studies to determine the red pigment has a maximum absorption peak at 505nm Department, Fermentation Monascus best days to 6~7 days,the appropriate medium for: rice flour 9%, NaNO3 0. 2%, KH2 PO4 0.1%, MgSO4 0. 2%. Stability of the red pigment found in red pigment at room temperature is relatively stable under the conditions,pH value of between 5 to 7 effects on the red pigment is relatively weak,biased towards extreme pH values of the red pigment stability is relatively large.。Indoor and outdoor effects of light on red pigment are not big.。Red pigment from the impact of common metal ions。Preservatives had no significant effect on red pigment,and not concentration。 Keywords:Monascus;Red Pigment ;Stability ;Extraction

  • 1,2,4-三氯苯的纯化和利用_制药工程论文范文

    制药工程论文范文 目 录 中文摘要I 英文摘要II 目录III 1. 绪论1 1.1 前言1 1.2 研究现状7 1.3论文研究内容及意义7 2. 实验部分8 2.1 实验仪器和试剂8 2.1.1 实验仪器8 2.1.2 实验试剂8 2.2 实验操作步骤9 2.2.1 废液的精馏9 2.2.2 精馏粗产物洗涤9 2.2.3 废液和精馏产物的硝化9 2.2.4 硝化产物还原10 3. 结果与讨论10 3.1 蒸馏馏分气相色谱分析10 3.2 洗涤产物气相色谱分析17 3.3 硝化剂用量对反应的影响17 3.4 不同还原剂对反应的影响19 3.5 讨论19 4.总结与展望20 4.1 总结20 4.2 展望20 致谢21 参考文献22 摘要:对2,4-二氯氟苯生产过程中所产生的废液三氯苯进行回收处理。通过废液分析可知其主要成分为2,4-二氯氟苯,并含有一定量的1,2,4-三氯苯及少量同分异构的三氯苯和多氯苯。首先通过精馏得到纯度为98%的2,4-二氯氟苯和纯度为88%的1,2,4-三氯苯,用洗洁精洗涤88%的1,2,4-三氯苯粗品,再用纯水清洗并干燥得到纯度为95%的1,2,4-三氯苯粗品,然后对95%的1,2,4-三氯苯进行硝化,得到99%的2,4,5-三氯硝基苯,并将所得产品还原成2,4,5-三氯苯胺。实验考察了不同的硝化方法、硝化剂的用量对反应的影响,研究结果表明:当粗产品用量为35ml、发烟硝酸为80ml时进行硝化,提纯后得到34.046g 2,4,5-三氯硝基苯,纯度为99.4%,而其还原产物2,4,5-三氯苯胺的纯度可达到99%。 关键词:2,4-二氯氟苯,1,2,4-三氯苯,提纯,硝化,还原,2,4,5-三氯苯胺 Abstract: This topic was about recycling of trichlorobezene from the preparation of 2,4-dichlorofluobezene. As the analysis of the recycling liquid showed, 2,4-dichlorofluobezene was the main part, and there was also some 1,2,4-trichlorobenzene and a little of isomers of trichlorobenzene and polychlorobezene. Firstly, 2,4-dichlorofluobezene and 1,2,4-trichlorobenzene were gained by distiling with the purity of 98% and 88%, respectively. Then 1,2,4-trichlorobenzene with the purity of 95% was got by cleaning with detergent and water. Thirdly, 2,4,5-trichloronitrobenzene was prepared by nitration from 1,2,4-trichlorobenzene, with the purity of 99%. finally, 1,2,4-trichlorobenzene was converted to 2,4,5-trichloroaniline by reduction. Different methods of nitration and amount of nitrating reagent were tested in this article. As the result showed, when nitration took place with 35ml of 1,2,4-trichlorobenzene and 80ml of fuming nitric acid, 36.046g of 2,4,5-trichloronitrobenzene was gained, with the purity of 99,4%, and the purity of its reducing production could reached 99%. Key words: 2,4-dichlorofluorobenzene, 1,2,4-trichlorobenzene, Purification, nitration, reduction, 2,4,5-Trichloroaniline

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