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腈基化合物的还原反应工艺研究和设计

时间:2021-09-23 21:32来源:毕业论文
在新型抗凝血药物的研究过程中的中间产物一类腈基化合物,通过Pinner反应生成脒类中间体(3-[4-(4-甲脒基-苯基氨基甲酰基)-苯基氨基]-丙酸乙酯)的反应过程及工艺优化

摘要:心脑血管疾病是一种有着较高死亡率的疾病,高血脂、高血压、血液粘稠和动脉硬化等常常威胁着中老年患者的健康,抗凝血药物能够有效防止血管内血栓的形成、缓解血液的凝固,对各种心脑血管疾病都有着很好的预防和治疗效果。72175

由于传统的抗凝血药物在治疗效果上有较多缺陷,近年来开发抗凝效果好、安全性高的新型抗凝血药物成为了研究热点。脒及其衍生物在医药与农药等方面都应用广泛,常常作为合成过程中重要的中间体应用在新型抗凝血药物的合成中,并对凝血酶有较好的抑制作用。过去在合成脒的传统工艺上存在着效率低、产率差、反应不易控制、投料复杂等缺点,近年来催化合成脒的工艺有了较大的进步,其合成路线也得到了简化。

本次课题主要研究的是在新型抗凝血药物的研究过程中的中间产物一类腈基化合物,通过Pinner反应生成脒类中间体(3-[4-(4-甲脒基-苯基氨基甲酰基)-苯基氨基]-丙酸乙酯)的反应过程及工艺优化。反应是由上一步产物与盐酸羟胺、无水乙醇、三乙胺、甲酸铵反应,以Pd/C为催化剂,合成了中间体脒,并考察了物料比、温度和反应时间对反应的影响,得到的最佳工艺条件:(1)在醇解反应步骤,盐酸羟胺与三乙胺的物料比为1:1,反应时间3h;(2)在胺解反应步骤,反应温度120℃,Pd/C催化剂浓度10%,反应时间5h,收率为82。7~85。2%。并通过核磁、质谱等对相关表征进行了分析。

毕业论文关键词:脒基;氰基还原;抗凝血;pinner法;工艺设计。

Research and Design of Reduction Reaction Process for a class of Nitrile Compounds

Abstract: Cardiovascular and cerebrovascular disease is a disease with a relatively high mortality rate。 The middle-aged and elderly are often under threat of Hyperlipidemia, hypertension, high blood viscosity and arteriosclerosis。 Anticoagulant drugs can effectively prevent the formation of intravascular thrombosis, relieve blood coagulation, and have good prevention and treatment effect for a variety of cardiovascular and cerebrovascular diseases。 

Because the traditional anticoagulant drugs have many defects in treatment effect, in recent years, to develop new types of anticoagulant drugs of good effect and high safety has become a research hotspot。 Amidine and its derivatives are widely used in medicine, pesticide and other fields。 Amidine compounds are often used as important intermediates in the synthesis process of new anticoagulants drugs, and have a good inhibitory effect on thrombin。 In the past, the traditional process of amidine formation has the disadvantages of low efficiency, low-yield, uncontrollability and complicated feeding; in recent years, the process of Catalytic synthesis amidine has made great progress, and the synthesis route has been simplified。

This research mainly study about the reaction process and process optimization of A class of nitrile compounds, the intermediate product in the research of new anticoagulant drugs, through the Pinner reaction to form Amidine intermediates(3-[4-(4-Carbamimidoyl-phenylcarbamoyl)-phenylamino]-propionic acid ethyl ester)。The reaction is carried out by reacting the previous product with hydroxylamine hydrochloride, anhydrous ethanol, triethylamine and ammonium formate, catalyzed by Pd/C。 Amidine intermediates is produced。 By studying the effects of material ratio, temperature and reaction time on the reaction, optimal technological conditions were discovered: (1) in the alcoholysis reaction, the ratio of hydroxylamine hydrochloride to triethylamine is 1: 1; the reaction time is 3h。 (2) in the amination reaction, the reaction temperature is 120 ℃; The concentration of Pd / C catalyst is 10%; the reaction time is 5 h; and the yield is 82。7~85。2%。 The related characterization was analyzed by nuclear magnetic resonance and mass spectrometry。 腈基化合物的还原反应工艺研究和设计:http://www.youerw.com/huaxue/lunwen_82066.html

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