文档介绍：南京理工大学硕士学位论文间甲苯胺合成间氟苯甲醛的研究姓名:孙卫芬申请学位级别:硕士专业:应用化学指导教师:吕春绪 20070601 南京理工大学硕士学位论文间甲苯胺合成问氟苯甲醛的研究摘要问氟苯甲醛是一种重要的医药工业原料,可用于合成新型抗生素喹诺酮类化合物,合成治疗高血压药,合成一些消炎药。本文以间甲苯胺为原料通过希曼反应制备间氟甲苯,再由间氟甲苯控制氧化合成间氟苯甲醛。在传统希曼反应的基础上改进工艺,加入三氯甲烷作为溶剂有效降低了重氮化反应的剧烈程度,通过因素分析得到了最佳反应条件如下:问甲苯胺与盐酸的最佳投料比(摩尔比)为l:,,重氮盐与三氯甲烷的质量比约为1:3, 在此条件下反应,%,%。分别采用了NHPI/Mn单金属体系、Co/Mn/Br无水体系控制氧化间氟甲苯,通过因素分析得到两种体系的最佳反应条件,%,%,%。对Co/Mn/Br体系控制氧化问氟甲苯反应机理进行了推测。并通过气质分析、红外分析、核磁分析鉴定其结构。关键词:问氟甲苯间氟苯甲醛希曼反应液相氧气氧化南京理工大学硕士学位论文问甲苯胺合成伺氟苯甲醛的研究 Abstract M-zaldehyde iS allimportant medication rawmaterial。which callbe usedforthe pounds antibioticofketone’S,the medicine Ofcure hi【gh blood pressure,and some diminishinflammation medicines. The article thesynthesis ofthe m-fluorobenzaldehyde with therawmaterialof m-,m-aminotoluene was applied toprepare m-fluorotoluene by Balz-Schemann reactionwith sodiunl nitriteand sodiunl fluoroborate,then m-fluorobenzaldehyde was achieved byliquidphase oxidation ofm-fluorotoluene. Inorder toimprove the订aditional craftwork ofBalz-Schemann reaction,chlorofc'Fin Wasaddedas solventtoeasethe whole conditions were obtained by theanalysis ofseveralparameters:the ratioofm-aminotoluene and hydrochloric acidWas1:(mole ratiobasedon),the amount ofsodium nitrite was ,the ratiooftetrafluoroboratesand chloroforln was about1:3(mass ratiobasedon).Under theseconditions,theyield canle %,the purity came %.Thearticle toldtwocatalystsystems fortheliquid phase oxidationofm-fluorotoluene,NHPF MnCl2 catalystsystemand Co(OAch/MnS04/KBr conditions wereobtainedby theanalysis ofseveral theoptimum conditions,the conversion of m-fluorotoluene came ,the selectivity came %,and theyield was %.Itspeculated onthemechanism ofCo(OAe)z/MnS04/KBr structure pounds Wasidentifiedby ,IR and1HNMIL Keywords:M-fluorotolue