Synthesis and Characterization of Polyaspartimides Containing Anisyl Moiety

New class of aromatic bismaleimides containing anisyl group were synthesized from bis(4-amino 3,5-dimethyl phenyl) anisyl methane and maleic anhydride via bismaleamic acid as an intermediate followed by cyclodehydration to bismaleimides. The structure was confirmed by FTIR, ¹H-NMR and elemental analysis. Further, a series of polyaspartimides were synthesized by addition reaction of bismaleimide (BMDA) with various diamines. The polymers were characterized by IR and elemental analysis. The polymers exhibit good solubility in organic solvents such as NMP, DMF and DMSO. They exhibit good thermal stability. T _g of polyaspartimides are in the range of 125–278°C and T _10% weight loss are in the range of 398–476°C.     

Synthesis and Characterization of Novel Polyamides Containing Purine Moiety

A series of new polyamides (inherent viscosities between 0.61 and 1.84?dL?g^?1) were prepared directly by low-temperature polycondensation of a new purine-moiety-containing diamines, 7,10-bis(4-aminopheny) adenine, with various acyl dichlorides in N-methyl-2-pyrrolidinone. The resultant polymers showed glass transition temperatures between 312–339°C and 5% weight loss temperatures ranging from 405 to 513 and 378 to 485°C in nitrogen and air atmosphere, respectively. Some polymers were amorphous and could be cast into transparent, light-colored, and flexible films with tensile strengths of 84–110?MPa, elongations at break of 8.4–16.5%, and tensile modulus of 3.3–5.5?GPa.     

Synthesis and Characterization of New Functional Polystyrenes Containing Tributyltin Carboxylate Moieties Linked to the Aromatic Ring by a Trimethylene Spacer

A novel trialkyltin carboxylate monomer, tributyltin 4-(p-styryl)-butanoate, characterized by the presence of a trimethylenic spacer linking the tin carboxylate moiety to the aromatic group, has been prepared and submitted to radical homo- and copolymerization with styrene in order to obtain the corresponding copolymers with variable contents of organometallic moiety. For the sake of comparison, tributyltin 4-(4-isopropylphenyl)-butanoate has also been synthesized as the structural model of the repeating unit of the polymers. All the products prepared have been characterized both in solution and in the solid state by spectroscopic and thermal techniques with the aim to establish the coordination state of the tin atom, a feature which is of importance for future application of these derivatives.     

含吲哚基1,3,4-噻二唑双腙的合成

冰乙酸为催化剂,2,5-二肼基-1,3,4-噻二唑与取代吲哚-3-甲醛在乙醇中缩合反应,得到了4种新型含吲哚基的1,3,4-噻二唑类双腙化合物,其结构经IR,1 H NMR所证实。最佳反应条件为:反应温度90℃,n(2,5-二肼基-1,3,4-噻二唑)∶n(取代吲哚-3-甲醛)=1.0∶2.4,反应时间4h,收率75.5%~81.0%。     

含噻唑环核肟酯类化合物的合成及生物活性研究

利用醛(酮)肟与2-氯-4-取代-5-噻唑甲酰氯反应,合成了8个含2-氯-4-取代噻唑环核的肟酯类化合物,所有化合物的结构均经1H NMR,13C NMR及元素分析确证。离体杀菌活性测试结果表明,目标化合物有一定的杀菌活性。     

含苯并咪唑的芳香族聚酰胺共聚物的合成与表征

采用低温溶液缩聚法,在N-甲基吡咯烷酮(NMP)-氯化锂(LiCl)溶剂体系中加入2-(4-氨基苯基)-5-氨基苯并咪唑(DAPBI)作为第三单体,与对苯二胺(PPD)和对苯二甲酰氯(TPC)共聚得到改性对苯二甲酰对苯二胺(PPTA)共聚物。控制共聚单体投料顺序,设计合成出一系列序列结构不同的杂环段与PPTA硬段相间的嵌段聚合物。研究了序列结构和DAPBI含量对共聚物比浓对数黏度的影响,采用红外光谱、X射线衍射、热重分析仪等对共聚物结构和性能进行表征。试验结果表明:DAPBI成功引入到了PPTA分子链中,改性PPTA树脂为非晶结构,所得有规嵌段共聚物比无规共聚物拥有更好的有序性和结晶性能,共聚物能保持良好的耐热性能,溶解性能和力学性能得到了提升。     

新型含萘环双马来酰亚胺三嗪树脂的合成、固化反应及其热性能的研究

合成出了新型含有萘环和醚键结构的双马来酰亚胺和氰酸酯单体,通过元素分析(EA)、傅立叶变换红外光谱(FT-IR)及核磁共振(1H-NMR)等手段对其进行表征分析,同时,用差示扫描量热法(DSC)、原位FT-IR对新型BMPN/DNCY树脂体系的共固化反应机理以及固化物结构进行了研究,并采用热失重法(TGA)分析该树脂在氮气条件下的耐热性能.研究结果表明,采用文中使用的方法合成出了高纯度、高产率的新型双马来酰亚胺和氰酸酯树脂单体;BMPN/DNCY树脂的固化反应主要是以BMPN/DNCY共聚反应生成两种六元环结构的共聚物为主,兼有少量BMPN单体自聚;在耐热性能方面,共固化所得双马来酰亚胺三嗪树脂的热分解起始温度(Tc)都在440℃以上,具有很好的热稳定性;不同配比的共固化结构双马来酰亚胺三嗪树脂热分解的Tc差别不是很大,在700℃时的残炭率都在60%左右.     

含受阻胺结构的苯并三唑光稳定剂的合成及表征

以3-(3′-叔丁基-4′-羟基-苯基)丙酸和邻硝基苯胺或邻硝基对氯苯胺为起始原料经重氮化-偶合、还原、酯化,再与甲基哌啶醇酯交换反应合成了4个分子中含受阻胺结构的苯并三唑化合物,2,2,6,6-四甲基哌啶醇-[3′-(2H-苯并三唑)-5′-叔丁基-4′-羟基-苯基]丙酸酯收率为48.3%;1,2,2,6,6-五甲基哌啶醇-[3′-(2H-苯并三唑)-5′-叔丁基-4′-羟基-苯基]丙酸酯收率为47.0%;2,2,6,6-四甲基哌啶醇-[3′-(5-氯-2H-苯并三唑)-5′-叔丁基-4′-羟基-苯基]丙酸酯的收率为45.7%;1,2,2,6,6-五甲基哌啶醇-[3′-(5-氯-2H-苯并三唑)-5′-叔丁基-4′-羟基-苯基]丙酸酯的收率为44.4%;通过1HNMR、MS和IR确定了化合物分子结构。测定了它们紫外吸收光谱,该4个化合物在270～400nm均有较强的吸收峰。所合成的化合物分子中同时含有紫外吸收和捕获自由基两种功能,是一类双功能光稳定剂。     

Synthesis and Characterization of Water-Soluble Metal Binding Polyesters Containing Pendant Carboxylic Moiety

The water-soluble polyesters were synthesized by the polyaddition reaction between diethylenetriaminepentaacetic acid bisanhydride (DTPABA) and polyethylene glycols (PEG) of different molar masses. The copper complexes of these polyesters were synthesized by the reaction with copper acetate and were characterized by their melting points, elemental analyses, viscometry, FT-IR, UV-visible SEM, AFM, XRD data. Thermal stability of the compounds was studied by TG-DTA analyses. The antibacterial activity of the polyesters was studied against the bacterial species E. coli, S. aureus, P. aeruginosa and B. subtilis. All the polyesters showed moderate anti-bacterial activity against the selected bacteria.     

Synthesis and Preliminary Cancer Activity of Chelidonic Acid Polyesters Containing the Triphenylarsenic,Triphenylantimony, and Triphenylbismuth Moiety

Polyesters derived from the interfacial reaction of the salt of chelidonic acid and triphenylarsenic dibromide, triphenylantimony dichloride, and triphenylbismuth dichloride are formed in moderate yield using commercially available reactants. IR data shows new bands characteristic of the formation of the M-O bond. MALDI MS shows formation of ion fragment clusters to two units. The polymers were tested for their ability to inhibit prostate, colon, breast (two cell lines), and pancreatic (two cell lines) cancer cells. All polymers showed ability to inhibit some of the cancer cell lines. The arsenic polymer exhibits good inhibition of the AsPC-1 pancreatic cell line. All three polymers inhibit the estrogen independent 7233 cell line to a much greater extent compared to inhibition of the 7259 estrogen positive receptor cell line. The arsenic and bismuth polymers also exhibit decent inhibition of the other cancer cell lines while the antimony polymer shows only decent inhibition of the 3465 prostate cell line.     

含吡啶环的双酰基硫脲衍生物的合成与生物活性

采用相转移催化法合成了6个含吡啶的双硫脲类新的化合物,其结构经1H NMR、IR、MS和元素分析表征。生物活性测试结果表明所设计化合物具有一定的植物生长调节活性。     

Synthesis, Characterization and Properties of Some Main-Chain Ferrocene-Based Polymers Containing Aromatic Units

Four main-chain ferrocene-based polymers containing aromatic units, including poly(o-Cresolphthalein 1,1′-ferrocene dicarboxylate) (PCPFD), poly(cresol red 1,1′-ferrocene dicarboxylate) (PCRFD), poly(2,4-quinolinediol 1,1′-ferrocene dicarboxylate) (PQDFD), and poly(sudan orange G 1,1′-ferrocene dicarboxylate) (PSOFD), were successfully synthesized. The solution polycondensation reaction was employed for the synthesis of PCPFD and PCRFD while PQDFD and PSOFD were synthesized via an interfacial polycondensation reaction. The synthesized polymers were characterized by ¹H and ¹³C NMR, UV–VIS absorption and FTIR spectra and X-ray diffraction. The synthesized main-chain ferrocene-based polymers are generally amorphous. The effect of organic solvent, scan rate, electrolyte concentration and [Fe] concentration on the cyclic voltammetric behavior of the synthesized polymers were examined. The thermal properties were investigated employing thermogravimetric analysis. The results revealed the relative thermal stability of the polymers. The liquid crystalline properties were studied. The results indicated that the synthesized polymers exhibited nematic phases during the scan cycles of heating and cooling with high phase duration.     

含硅氢基团甲基芳炔树脂的合成及表征

以二氯甲基硅烷和间二乙炔基苯为原料,通过格氏反应合成了不同分子量的含硅氢基团甲基芳炔树脂(PSA-H),并分析确定了合成产物的结构. 树脂的热固化行为和固化树脂的热稳定性分析表明,PSA-H树脂具有良好的加工性能,可在较低的温度下(低于200℃)发生交联反应. 其固化物有较低的介电常数(2.57 F/m)、较低的介电损耗(tand 0.001)和优异的热稳定性,在N2气氛下5%失重温度Td5为675~703℃, 1000℃的残留率为90.9%~91.4%. PSA-H树脂固化物在氩气中1450℃下烧结可形成含b-SiC陶瓷.     

含芳酰胺键的液晶双马来酰亚胺的合成与表征

通过对马来酰亚胺基苯甲酸及其酰氯化路线合成了两种含芳酰胺键的液晶双马来酰亚胺Ⅰ b和Ⅱ b;制备了二苯甲烷二胺与液晶双马来酰亚胺Ⅱ b的扩键其聚物Ⅲb。经FTIR、~1H-NMR谱对合成产物的结构进行了表征,表明1710cm~(-1)的酰亚胺羰基和1646cm~(-1)酰胺键,交联反应或扩链反应发生在双马来酰亚胺的双键上。经热分析DTA/DSC及热台偏光显微镜表征了其热性能及液晶相变特征,相变过程是一个非平衡不可逆过程。     

含5-氨基噻唑环核双酰胺类化合物的合成及其生物活性

以商品化双酰胺基本骨架为先导,设计并合成了13个含5-氨基噻唑环核的苯甲酰脲类化合物,优化了基于Ugi四组件反应合成2,4-二取代-5-氨基噻唑中间体的方法,其结构均经1HNMR、13CNMR、IR和MS确证。初步离体杀虫活性测试结果表明:部分该类化合物具有很好的杀虫活性,当质量浓度为10 mg/L,化合物Ⅴf、Ⅴg、Ⅴh、Ⅴj和Ⅴm对蚊幼虫均显示100%的杀虫活性,且当质量浓度降至5 mg/L和2 mg/L时,化合物Ⅴj的杀虫活性仍有100%,高于阳性对照;当质量浓度为600 mg/L,化合物Ⅴd、Ⅴg对棉铃虫和玉米螟均显示100%的杀虫活性。     

含硒邻苯二甲酰胺类新化合物的合成、结构表征及杀虫活性

[方法]为获得新型鱼尼汀受体类杀虫剂,以3-碘苯酐及2-甲基-1-甲硒基-2-丙胺为起始原料,经缩合反应、关环及开环反应制备了系列含硒的邻苯二甲酰胺类新化合物(5a-5i,收率46%-50%),以核磁共振氢谱及元素分析等手段对中间体、终产物结构进行了表征。[结果]杀虫活性筛选表明化合物5a、5d、5h、5i在100 mg/L质量浓度下对小菜蛾杀死率达到90%以上。[结论]通过构效关系的分析得知:以先导物氟虫酰胺为对照,改变脂肪胺部分为含硒片段,活性总体下降;芳香胺的氨基对位为二氯烯丙氧基时,氨基邻位的卤原子对杀虫活性具有促进作用。     

2-甲基-4-硝基咪唑环修饰1,3,4-噁二唑的合成及抗菌活性研究

为研究和开发具有更高生物活性的1,3,4-噁二唑类候选化合物,以2-甲基-4-硝基-1-咪唑乙酸乙酯和芳香肼在丙基磷酸环酐作用下缩合反应制得的双酰肼为原料,对甲基苯磺酰氯为催化剂,设置微波功率为800 W,辐射时间为12~15min,通过环合反应制备2-甲基-4-硝基咪唑环修饰的1,3,4-噁二唑(4a~4i),合成收率为82%~92%,其结构经IR、1 H NMR和元素分析等测试技术得以证实。初步抗菌试验结果表明,目标化合物对大肠杆菌、金黄色葡萄球菌和枯草杆菌都有不同程度的抑制作用。     

对甲苯基双胍盐酸盐的合成及性能研究

以对甲苯胺为原料对双氰胺进行改性,合成了一种新型的改性双氰胺固化剂——对甲基苯基双胍盐酸盐。利用DSC方法考察了产物固化环氧树脂E-44体系的固化性能,结果表明,作为环氧树脂固化剂单独使用时,固化温度比双氰胺体系(180℃)降低了近60℃。确定固化工艺为80℃/2 h 100℃/1 h。     

Synthesis and Characterization of Tetra-Functional Epoxy Resins from Rosin

Tetra functional epoxy resins were prepared by the reaction of diethanolamine with Diels–Alder adducts of rosin ketone. These adducts were reacted with epichlorohydrine in the presence of NaOH as a catalyst to produce epoxy resins. The resins obtained were characterized by IR and ¹H NMR spectroscopy. The curing behaviours of these resins with their poly (amide-imide) derivatives were investigated by viscosity measurements. The curing activation energy was calculated from the gel time and critical viscosity measurements. The curing exotherms of the epoxy resins produced with poly (amide-imide) hardeners were investigated. The curing and gel times of the resins produced show slight differences between the synthesized resins. The chemical resistances and mechanical properties of the cured films were evaluated. The produced coats show high stability for salt spray at a duration time of 563 h.