药物合成实验讲义

不排除由于是进行产品质量评审时,在项目的设置、抽样方法与质量检验的严谨程度上,都尚存在一定的问题；所以产品评审的过程需要进一步改进；以便更真实地反映情况出产品的真实问题；从而更全面、更本质地反映产品质量存在的问题与真实水平centerpinchecksandanchoringtheinnercylinder.AccordingtoWhilecouplingalignmentshouldkeepoiloutofcavityandlocatetherotoraxisneckraisedarewithintheprescribedlimits,thereshouldbenogaps,Horn,HornandHorn0.05mmfeelergaugesfitinto.Centercoupling,condenserwaterfillingandwater-filledaccordingtofactoryrequirement.ForcouplingthreesupportedrotorCenter,themouthunderthecouplingbetweenthevalueshouldbeasstipulatedinthemanufacturer,usually0.15~0.25mm.Inthecaseofcouplingconnection,ifpossible,liftingonlyonebearingendofthesupportbearingoftherotor,removethebearing,fittedwithspecialtilesandspecialliftingtools,discrotors,checkthejournalfluttertile,shouldgenerallybelessthan0.10MM.Whenthecouplingsandrotorcomeswhenthereisaconflict,thecouplingCentreshallprevail.6.4.5.2.2shaftlookingfor:...6.4.5.3.Provisionalboltconfirmedthepositioningoftherotorsize,aswellasthecouplingbetweentheadjustmentshimthicknessaccuracy,drawingstomeetthetechnicalrequirements.Plane,cylindricalandcleanthecouplingboltholesshouldbecleanandwithoutburrs,scrapironandgrease-free,relativepositionofthecouplingaccordingtothedrawingrequirementsare.Couplingtopscrews,rounddistanceapart,indicatorstomonitormovementoftheaircraft,itsvalueisallowedtopassthevalueaxismoving,mountedadjustmentpads,notepadsinstallationdirectionguidepincouplingwithprocessendclosed.Thebackwheelsslowlytightened,when2mmorso,withstandardwhitebarswheretwobackwheelboltholemeasurementaboveandbelow,confirmtwobackwheelboltholeconcentricity.Then,thesymmetricalhorizontalmounttwotemporaryboltstightened,attentiontomonitordialindicator,theninstallthesymmetricaltemporarybolts,thistimesitesslowlymovingrotor,inthemeasuredcircumferenceof8equalpartsbackwheelrimrock,eachmeasuringrelativechangesinvalueshouldbelessthan0.02mm.6.4.5.4couplingreamedandpairedboltreamingdiereamer,adjustablereamers,boringmill,inseveralways.6.4.5.4.1Generalrequirementsbeforereamingorboring,药物合成实验讲义湛江师范学院化学科学与技术学院2011年2月20目录实验一阿司匹林的合成………………………………………………………………2实验二扑炎痛的合成…………………………………………………………………3实验三水杨酰苯胺的合成……………………………………………………………5实验四苯佐卡因的合成………………………………………………………………7实验五利尿药氯噻酮中间体的合成………………………………………………9实验六维生素K3的合成……………………………………………………………10不排除由于是进行产品质量评审时,在项目的设置、抽样方法与质量检验的严谨程度上,都尚存在一定的问题；所以产品评审的过程需要进一步改进；以便更真实地反映情况出产品的真实问题；从而更全面、更本质地反映产品质量存在的问题与真实水平centerpinchecksandanchoringtheinnercylinder.AccordingtoWhilecouplingalignmentshouldkeepoiloutofcavityandlocatetherotoraxisneckraisedarewithintheprescribedlimits,thereshouldbenogaps,Horn,HornandHorn0.05mmfeelergaugesfitinto.Centercoupling,condenserwaterfillingandwater-filledaccordingtofactoryrequirement.ForcouplingthreesupportedrotorCenter,themouthunderthecouplingbetweenthevalueshouldbeasstipulatedinthemanufacturer,usually0.15~0.25mm.Inthecaseofcouplingconnection,ifpossible,liftingonlyonebearingendofthesupportbearingoftherotor,removethebearing,fittedwithspecialtilesandspecialliftingtools,discrotors,checkthejournalfluttertile,shouldgenerallybelessthan0.10MM.Whenthecouplingsandrotorcomeswhenthereisaconflict,thecouplingCentreshallprevail.6.4.5.2.2shaftlookingfor:...6.4.5.3.Provisionalboltconfirmedthepositioningoftherotorsize,aswellasthecouplingbetweentheadjustmentshimthicknessaccuracy,drawingstomeetthetechnicalrequirements.Plane,cylindricalandcleanthecouplingboltholesshouldbecleanandwithoutburrs,scrapironandgrease-free,relativepositionofthecouplingaccordingtothedrawingrequirementsare.Couplingtopscrews,rounddistanceapart,indicatorstomonitormovementoftheaircraft,itsvalueisallowedtopassthevalueaxismoving,mountedadjustmentpads,notepadsinstallationdirectionguidepincouplingwithprocessendclosed.Thebackwheelsslowlytightened,when2mmorso,withstandardwhitebarswheretwobackwheelboltholemeasurementaboveandbelow,confirmtwobackwheelboltholeconcentricity.Then,thesymmetricalhorizontalmounttwotemporaryboltstightened,attentiontomonitordialindicator,theninstallthesymmetricaltemporarybolts,thistimesitesslowlymovingrotor,inthemeasuredcircumferenceof8equalpartsbackwheelrimrock,eachmeasuringrelativechangesinvalueshouldbelessthan0.02mm.6.4.5.4couplingreamedandpairedboltreamingdiereamer,adjustablereamers,boringmill,inseveralways.6.4.5.4.1Generalrequirementsbeforereamingorboring,21实验一阿司匹林（Aspirin）的合成一、目的要求1.掌握酯化反应和重结晶的原理及基本操作。2.熟悉搅拌机的安装及使用方法。二、实验原理阿司匹林为解镇痛药，用于治疗伤风、感冒、头痛、发烧、神经痛、关节痛及风湿病等。近年来，又证明它具有抑制血小板凝聚的作用，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。阿司匹林化学名为2-乙酰氧基苯甲酸，化学结构式为：OCOCH3COOH阿司匹林为白色针状或板状结晶，mp.135~140℃，易溶乙醇，可溶于氯仿、乙醚，微溶于水。合成路线如下：OCOCH3COOHOHCOOH(CH3CO)2OH2SO4CH3COOH++三、实验方法（一）酯化在装有搅拌棒及球形冷凝器的100mL三颈瓶中，依次加入水杨酸10g，醋酐14mL，浓硫酸5滴。开动搅拌机，置油浴加热，待浴温升至70℃时，维持在此温度反应30min。停止搅拌，稍冷，将反应液倾入150mL冷水中，继续搅拌，至阿司匹林全部析出。抽滤，用少量稀乙醇洗涤，压干，得粗品。（二）精制将所得粗品置于附有球形冷凝器的100mL圆底烧瓶中，加入30mL乙醇，于水浴上加热至阿司匹林全部溶解，稍冷，加入活性碳回流脱色10min，趁热抽滤。将滤液慢慢倾入75mL热水中，自然冷却至室温，析出白色结晶。待结晶析出完全后，抽滤，用少量稀乙醇洗涤，压干，置红外灯下干燥（干燥时温度不超过60℃为宜），测熔点，计算收率。（三）水杨酸限量检查取阿司匹林0.1g，加1mL乙醇溶解后，加冷水定适量，制成50mL溶液。立即加入1mL新配制的稀硫酸铁铵溶液，摇匀；30秒内显色，与对于照液比较，不得更深（0.1%）。不排除由于是进行产品质量评审时,在项目的设置、抽样方法与质量检验的严谨程度上,都尚存在一定的问题；所以产品评审的过程需要进一步改进；以便更真实地反映情况出产品的