阿司匹林合成实验

阿司匹林合成实验 阿司匹林合成实验装置 说明书 天津大学化工基础实验中心 2013(8 poverty. In the area of poverty alleviation, to rely on e-commerce business park, active docking Alibaba group "rural treasure", "the stars plan" and "featured the Museum" project to accelerate the implementation of electronic commerce "hundred thousand rural village" project, free train operation staff, offering online support help for poor families, the provision of micro-credit support, helping them to use e-commerce platform to escape poverty. In poverty reduction, give a man a fish and feed him for a day, to targeted skills training and entrepreneurship training free of charge for the poor, increase employment, entrepreneurial skills, ensure the transfer of training people, poverty. In terms of student poverty, high school, vocational college students ' stipends and other costs, can be through the "one card", such as direct subsidies to households. In terms of financial poverty, in order to further increase the size of loans, expands the scope of delivery, developing industry, Enterprise provides protection for the poor. In respect of transport poverty alleviation, to solve the bottleneck in poor villages, development of transport, vigorously promoting the construction of rural roads and ordinary roads. PV poverty reduction, to support conditions of poor villages and photovoltaic system of centralized, poor construction projects, poor 一、实验目的 1(通过阿司匹林合成实验，了解酯化反应和精制原理，掌握其基本操作。 2(熟悉药物合成实验装置的结构组成、安装及使用。 二、实验内容 1(水杨酸与醋酐反应合成阿司匹林。 2(阿司匹林粗品精制。 3(水杨酸的限量检测。 三、实验原理 OCOCH3 阿司匹林(Aspirin)的化学结构式为: COOH 化学名: 2-(乙酰氧基)苯甲酸，又称乙酰水杨酸。 分子式: CHO 984 分子量: 180.16 性 状: 白色针状或片状结晶，无臭或微带醋酸臭，味微酸，遇湿气缓慢分解。熔点135~140?。易溶于乙醇，可溶于氯仿、乙醚，微溶于水。 早在18世纪人们就从柳树皮中提取出具有止痛、退热、抗炎的一种化学物质—水杨酸。但是由于水杨酸严重刺激口腔、食道和胃壁粘膜从而限制了其应用。为了克服这一缺点，人们在水杨酸分子中引入了乙酰基，即制备了乙酰水杨酸，又名阿司匹林(Aspirin)。 阿司匹林是一类解热镇痛药，用于治疗头疼、牙痛、肌肉痛、神经疼、关节疼等慢性钝痛及伤风、感冒、发烧等疾病，对风湿热及活动型风湿性关节炎等病疗效显著，是一种首选药物。近年的实验明它还可以抑制血小板中血栓烷A(TXA, 5-6) 合成，已知TXA有强大的血小板聚集及血栓形成的作用。高浓222 度阿司匹林能够抑制血管壁中环氧酶，减少TXA的合成，因而有抗血小板聚集2 及血栓形成的作用，其治疗范围又进一步扩大到预防血栓形成，治疗心血管疾患。本品有望发展成为心血管系统疾病的预防药。其主要副反应是会引起幽门痉挛及会引起刺激胃粘膜的胃肠道反应，长期服用有可能导致胃肠道出血。由于粗阿司匹林中会含有水杨酸及其它水杨酸衍生物如乙酰水杨酸酐、乙酰水杨酰水杨酸酯等，这些杂质具有免疫活性，可能导致服用阿司匹林的过敏反应，因此需要进行限量检查。 1centralized, poor construction projects, poorn of rural roads and ordinary roads. PV poverty reduction, to support conditions of poor villages and photovoltaic system of ructiosport poverty alleviation, to solve the bottleneck in poor villages, development of transport, vigorously promoting the constof loans, expands the scope of delivery, developing industry, Enterprise provides protection for the poor. In respect of transize ough the "one card", such as direct subsidies to households. In terms of financial poverty, in order to further increase the people, poverty. In terms of student poverty, high school, vocational college students ' stipends and other costs, can be thr iningntrepreneurship training free of charge for the poor, increase employment, entrepreneurial skills, ensure the transfer of traplatform to escape poverty. In poverty reduction, give a man a fish and feed him for a day, to targeted skills training and e commerce-credit support, helping them to use e-ration staff, offering online support help for poor families, the provision of microeum" project to accelerate the implementation of electronic commerce "hundred thousand rural village" project, free train opecommerce business park, active docking Alibaba group "rural treasure", "the stars plan" and "featured the Mus-poverty. In the area of poverty alleviation, to rely on e 本实验合成是以水杨酸为原料，在硫酸催化下，用醋酐乙酰化制得。 OHOCOCHHSO324 (CHCO)O32COOHCH3COOHCOOH 工艺流程: 四、实验装置的基本情况: 1.实验装置流程示意图: 冷却水 图、阿司匹林合成实验装置 加热器、冷凝管、热水泵、玻璃合成器、搅 拌桨、加料口、搅拌电机、温度计、恒温 槽、玻璃储槽、过滤介质、收集瓶、真空 表、调节阀、缓冲罐、真空泵。 2( 实验设备、仪器 药物合成实验装置包括:玻璃夹套反应釜、不锈钢恒温水槽、不锈钢真空缓冲罐、旋片式真空泵、搅拌电机、螺旋桨式搅拌器。 ages and photovoltaic system of centralized, poor construction projects, poorr vill, vigorously promoting the construction of rural roads and ordinary roads. PV poverty reduction, to support conditions of poofor the poor. In respect of transport poverty alleviation, to solve the bottleneck in poor villages, development of transportction in order to further increase the size of loans, expands the scope of delivery, developing industry, Enterprise provides protepends and other costs, can be through the "one card", such as direct subsidies to households. In terms of financial poverty, ' sti kills, ensure the transfer of training people, poverty. In terms of student poverty, high school, vocational college studentsto targeted skills training and entrepreneurship training free of charge for the poor, increase employment, entrepreneurial scommerce platform to escape poverty. In poverty reduction, give a man a fish and feed him for a day, -credit support, helping them to use e-village" project, free train operation staff, offering online support help for poor families, the provision of microaccelerate the implementation of electronic commerce "hundred thousand rural commerce business park, active docking Alibaba group "rural treasure", "the stars plan" and "featured the Museum" project to -rty. In the area of poverty alleviation, to rely on epove2 3(实验用试剂及仪器: 水杨酸、乙醇、醋酐、浓硫酸、烧杯、量筒、吸球等。 电机调速 合成器温度,?,干燥器温度,?, 总电源恒温器水泵恒温器加热 真空泵干燥器风机干燥器加热 图2、实验装置面板图 五、 实验步骤 1(酯化: (1)恒温水槽中加入纯水，开启水温控制，至所需温度备用。 (2)从反应釜进料口依次按量加入干燥的水杨酸120g，醋酐195 ml，浓硫酸9 ml。搅拌，混合均匀。 (3)开启恒温循环器加热，至反应釜中温度为70~75?。 (4)搅拌下保温约1小时左右。 (5)停止搅拌及保温。从反应釜中将的液体放入烧杯中，稍冷后向反应釜中加入冰水300ml。 (6)冷却到室温左右时，进行抽滤，得阿司匹林粗品。 2.精制: (1)调节恒温器加热，使反应釜内温度达到60?。 (2)向反应釜内加入300ml乙醇并将阿司匹林粗品放入反应釜中搅拌均匀使其溶解。倒出液体至烧杯中，加入粒状活性碳脱色3-5分钟，趁热过滤。 3centralized, poor construction projects, poorn of rural roads and ordinary roads. PV poverty reduction, to support conditions of poor villages and photovoltaic system of ructiosport poverty alleviation, to solve the bottleneck in poor villages, development of transport, vigorously promoting the constof loans, expands the scope of delivery, developing industry, Enterprise provides protection for the poor. In respect of transize ough the "one card", such as direct subsidies to households. In terms of financial poverty, in order to further increase the people, poverty. In terms of student poverty, high school, vocational college students ' stipends and other costs, can be thr iningntrepreneurship training free of charge for the poor, increase employment, entrepreneurial skills, ensure the transfer of traplatform to escape poverty. In poverty reduction, give a man a fish and feed him for a day, to targeted skills training and e commerce-credit support, helping them to use e-ration staff, offering online support help for poor families, the provision of microeum" project to accelerate the implementation of electronic commerce "hundred thousand rural village" project, free train opecommerce business park, active docking Alibaba group "rural treasure", "the stars plan" and "featured the Mus-poverty. In the area of poverty alleviation, to rely on e (3)将滤液倒入反应釜中并加入300 ml温水(40-50?)，将反应釜内温度逐渐下降冷却结晶，釜内析出白色结晶。 (4)抽滤，用少量冰水洗涤，干燥(常压干燥时温度不超过60?为宜)称重。 六、注意事项 1(安装时要小心、使用仪器设备动手要轻，特别注意不要打碎玻璃仪器。 2(水杨酸应当预先干燥、乙酸酐应使用新蒸的并且纯度较高;取用浓硫酸、乙酸酐的量筒和反应器也应提前干燥。 3(结晶母液系酸性液体，对皮肤以及眼睛具有刺激性和腐蚀性，应避免与皮肤直接接触，不慎粘上应及时用大量清水冲洗; 4(醋酐具有催泪性和腐蚀性，取用时必须带乳胶手套并在通风橱中进行，不慎粘上时，应及时用大量清水冲洗; 5(在初始加料混合时，水浴为室温或控制水温在30?下，以防止反应剧烈而冲料。 6(反应温度不宜过高，时间也不要太长，否则会增加副产物的生成。 7(用溶剂重结晶时溶液不宜加热过久，也不宜采用高沸点溶剂。因为乙酰水杨酸容易受热分解。 8(乙酰水杨酸受热后容易分解，分解温度为128~135?。熔点较难测定，在测定熔点时，可以先将热载体加热到120?左右后再放入样品测定。 9(水杨酸原料中可能混有苯酚等杂质，在制备阿司匹林过程中会产生乙酰苯酯和阿司匹林苯酯，它们在碳酸钠中不溶，故应检查阿司匹林在碳酸钠中的不溶性杂质。 10(本品在制备过程中，会由于反应不完全而带入未反应的水杨酸;在成品储存过程中，也会发生酯基的水解而产生水杨酸。水杨酸的存在不仅增加了对人体胃肠道的刺激，而且还较易氧化生成一系列醌式有色物质，这是阿司匹林不稳定变色的主要原因。 OCOOH[O]HOCOOH[O]COOHOHOHO 黄色 4ages and photovoltaic system of centralized, poor construction projects, poorr vill, vigorously promoting the construction of rural roads and ordinary roads. PV poverty reduction, to support conditions of poofor the poor. In respect of transport poverty alleviation, to solve the bottleneck in poor villages, development of transportction in order to further increase the size of loans, expands the scope of delivery, developing industry, Enterprise provides protepends and other costs, can be through the "one card", such as direct subsidies to households. In terms of financial poverty, ' sti kills, ensure the transfer of training people, poverty. In terms of student poverty, high school, vocational college studentsto targeted skills training and entrepreneurship training free of charge for the poor, increase employment, entrepreneurial scommerce platform to escape poverty. In poverty reduction, give a man a fish and feed him for a day, -credit support, helping them to use e-village" project, free train operation staff, offering online support help for poor families, the provision of microaccelerate the implementation of electronic commerce "hundred thousand rural commerce business park, active docking Alibaba group "rural treasure", "the stars plan" and "featured the Museum" project to -rty. In the area of poverty alleviation, to rely on epove OOHOOHOOHO+或+OHOOOCOOHCOOHCOOHCOOHCOOHCOOH 蓝至黑色 七、报告内容 1(实验名称、实验目的、实验原理 2(实验:时间、操作步骤、现象、温度等，并记录熔点、最终产品量及计算收率。 3(实验结果与讨论 5centralized, poor construction projects, poorn of rural roads and ordinary roads. PV poverty reduction, to support conditions of poor villages and photovoltaic system of ructiosport poverty alleviation, to solve the bottleneck in poor villages, development of transport, vigorously promoting the constof loans, expands the scope of delivery, developing industry, Enterprise provides protection for the poor. In respect of transize ough the "one card", such as direct subsidies to households. In terms of financial poverty, in order to further increase the people, poverty. In terms of student poverty, high school, vocational college students ' stipends and other costs, can be thr iningntrepreneurship training free of charge for the poor, increase employment, entrepreneurial skills, ensure the transfer of traplatform to escape poverty. In poverty reduction, give a man a fish and feed him for a day, to targeted skills training and e commerce-credit support, helping them to use e-ration staff, offering online support help for poor families, the provision of microeum" project to accelerate the implementation of electronic commerce "hundred thousand rural village" project, free train opecommerce business park, active docking Alibaba group "rural treasure", "the stars plan" and "featured the Mus-poverty. In the area of poverty alleviation, to rely on e