2,4-二甲氧基苯甲酰氯的合成

2,4-二羟基苯甲酸与硫酸二甲酯经甲基化反应得到2,4-二甲氧基苯甲酸(3);3与SOCl2发生氯化反应合成了2,4-二甲氧基苯甲酰氯(4)。较佳的氯化反应条件为:325mmol,苯70mL,AlCl3250mg,回流反应1.5h,重结晶溶剂为石油醚(90℃～120℃),总产率达74.1%。2～4的结构经1HNMR和FT-IR表征。     

SYNTHESIS AND-CHARACTERIZATION OF THE SOLUBLE, HIGH MOLECULAR WEIGHT AND LADDERLIKE POLYHYDROSILSESQUIOXANE AND ITS COPOLYMERS

The high molecular ladderlike polyhydrosilsesquioxane (LPHSQ) and its copolymer, ladderlike random copolymethylhydrosilsesquioxane (LR-PMHSQ) and ladderlike block copolymethylsilsesqui-oxane(LB-PMHSQ) have been synthesized by a preaminolysis reaction of the corresponding trichlorosilane with 1 ,4-phenylene diamine(PDA) then by hydrolysis and polycondensation reactions The thermographs of these polymers measured by DSC method indicate that these macromolecular backbones are very rigid as seen from the DSC curves which are almost horizontal from room temperature until 350 ~C without noticeable glass transition. The content of Si—H group in the polymers can be regulated by changing the composition of the two copolymerized monomers. So the ladderlike polymers including its copolymers can be the useful precursors for the functional polymers, especially such as fishbone-like liquid crystalline polymers.     

高规整梯形聚乙烯基倍半硅氧烷的合成

采用具有"同步增长,同步断撑和原位缩合"特性的超分子构筑调控逐步偶联和聚合方法,合成了高规整的反应性梯形聚乙烯基倍半硅氧烷Vi-LPSQ.该反应性乙烯基可进一步功能化,是制备功能高分子材料的重要前驱体.29Si-NMR是表征梯形聚合物规整性最有效的方法,Vi-LPSQ的重复结构单元共振吸收峰的化学位移δ=-21.6,且峰宽Δca.1,说明其规整性很高.它的XRD谱图上存在两个明显的衍射峰,分别对应于梯形的宽度(d1=0.74 nm)和厚度(d2=0.40 nm),这证实了Vi-LPSQ以典型的梯形结构存在.另外,Vi-LPSQ的玻璃化转变温度Tg高达191.3℃,表明Vi-LPSQ分子具有很高的刚性和规整性.     

一种含二茂铁的有机分子在超高密度信息存储中的应用研究

通过缩合反应合成了含二茂铁的有机给受体分子1-二茂铁基-2-(4-对硝基苯基)亚胺,利用真空沉积的方法制备了其薄膜,观察了该薄膜形貌,测定了其电学特性。结果发现,该薄膜具有良好的电学双稳态。利用STM成功地在该薄膜上写入了纳米尺度信息点。这一结果表明,该分子可望作为一种具有潜力的超高密度信息存储材料。     

9,10-二(4-烷氧基苯乙烯基)蒽衍生物的合成及其荧光性质

以蒽环为中心核,由中间体对烷氧基苯甲醛与9,10-二(亚甲基亚磷酸二甲酯)蒽通过Arbusov-Horner反应,合成了4个9,10-二(4-烷氧基苯乙烯基)蒽衍生物(4a～4d),其结构经1H NMR和FT-IR表征.对4的荧光性质进行了初步研究,结果表明:随着柔性链碳原子数目的增加,其荧光强度逐渐增强,4a～4d的最大荧光发射波长分别为525 nm,523 nm,517 nm和515 nm.     

LADDER SUPERSTRUCTURE-DIRECTED SYNTHESIS OF A WELL-DEFINED m-PHENELENEDIIMINO-BRIDGED LADDER POLYMETHYLSILOXANE

A well-defined m-phenylenediimino-bridged ladder polymethylsiloxane(LP) was first synthesized through a welldefined ladder superstructure(LS) acting as synthetic template,which was self-assembled by concerted interaction of hydrogen bonding and aromaticπ-πstacking of the monomer(M),N,N'-bis(phenyldichlorosilyl)-m-phenylenediamine.Some key characterization data of LP and,in particular,the extremely vulnerable LS with very unstable Si-Cl and Si-N groups were given.The molecular weights(M_n) of LS and LP ar...