N-羟基丁二酰亚胺的制备

本文介绍了制备N-羟基丁二酰亚胺的一般方法，研究了制备N-羟基丁二酰亚胺水合物的工艺方法，以及从一水合N-羟基丁二酰亚胺出发制备高纯度无水N-羟基丁二酰亚胺的方法。     

N-羟基丁二酰亚胺的合成工艺研究

目的：文章旨在对于传统工艺进行简化,提高产率,得到先进的工艺合成技术。方法：研究采用真空脱水法制备高纯度N-羟基丁二酰亚胺。结果：对反应过程的工艺条件进行研究,通过单因素实验和正交实验找到了最佳工艺参数。结论：确定了合成N-羟基丁二酰亚胺的最佳工艺过程。     

N羟基丁二酰亚胺的合成

介绍了Ｎ－羟基丁二酰亚胺的两种合成方法，并进行了比较，认为方法二可行。     

水中苯胺类化合物检测8-羟基喹啉试剂盒的研制

本文提出一种能方便、快速、灵敏地检测水中苯胺类化合物的试剂盒。该方法是以N -氯代丁二酰亚胺和 8-羟基喹啉与苯胺的显色反应为基础。显色反庆所得的蓝绿色化合物的最大吸收波长为 6 1 0nm ,在苯胺为 0 .2～ 8mg/L的浓度范围内符合比尔定率 ,最低检出限为 0 .0 1mg/L ,测定的重现性在± 5 %以内。本方法已成功地用于环境水样的分析测定     

国内专利文献

9-芴甲氧羰酰丁二酰亚胺酯的纯化工艺;四苯甲烷衍生物及其应用;N,N’-二环已基碳二亚胺生产工艺;α-氰基丙烯酸酯的制备方法;连续制备异氰酸酯的方法;2-辛基-3,4-二（7-异氰酸酯庚基）-1-己基环己烷及其制备方法和用途     

N-羟基丁二酰亚胺合成研究

研究了采用一步法合成N-羟基丁二酰亚胺的工艺,并对各种反应条件进行了研究。当反应温度40℃,n盐酸羟胺∶n丁二酸酐为1∶1.2,高真空除水,合成收率达75.3%,产品纯度≥99.5%。     

乳化炸药用聚异丁烯丁二酰亚胺热合法探究

介绍了乳化炸药用聚异丁烯丁二酰亚胺热合原理及工艺流程。对氯化法和热合法生产的聚异丁烯丁二酰亚胺在粉状乳化炸药中的使用效果作了比较。     

新型聚异丁烯丁二酰亚胺乳化剂的合成及其性能

以聚异丁烯丁二酸酐,N-羟乙基-乙二胺为主要原料,合成了新型聚异丁烯丁二酰亚胺乳化剂产品,并用红外光谱对其进行结构表征。测定了产品的乳化性能与储存稳定性能,结果表明,所合成的新型聚异丁烯丁二酰亚胺乳化剂的乳化性能与储存稳定性能均优于聚异丁烯丁二酰亚胺(T152)以及聚异丁烯丁二酸聚甘油酯乳化剂,适用于乳化炸药行业。     

N-溴代丁二酰亚胺绿色合成工艺条件的探究

以溴酸钠、溴化钠、硫酸、丁二酰亚胺为主要原料,研究了N-溴代丁二酰亚胺(NBS)的绿色化合成工艺。优化工艺条件为:原料配比n(溴酸钠)∶n(溴化钠)∶n(硫酸)∶n(丁二酰亚胺)=1∶2∶1.7∶2.6,溶剂水90 mL,反应温度为20~40℃,反应时间为2.5 h,此条件下产品收率87%,有效溴含量为44.3%,纯度98.6%。     

丁二酰亚胺在乳化炸药中的应用研究

研究了聚异丁烯丁二酰亚胺作为乳化炸药乳化剂的技术特点,并同常用乳化剂司苯 80作了比较。研究表明,以聚异丁烯丁二酰亚胺作为乳化剂的乳化炸药,具有小而分布均匀的W/O粒子,较强的稳定性及良好的爆炸性能。     

Bioinspired and biocompatible adhesive coatings using poly(acrylic acid)‐grafted dopamine

Poly(acrylic acid) (PAA) was grafted with dopamine to increase its adhesion force to metal surface. Nitinol plate surfaces were then modified by coating with PAA‐g‐dopamine. To synthesize PAA‐g‐dopamine, PAA was first activated by dicyclohexylcarbodiimide and N‐hydroxysuccinimide (NHS) to form PAA–NHS. Dopamine was then copolymerized with PAA–NHS in an aqueous medium at pH 8.5. We propose to increase the adhesion of adhesive PAA‐g‐dopamine on nitinol to improve its durability. In this article, we studied wettability, surface elemental composition, and surface morphology. Biocompatibility was also assessed by L929 fibroblast cells in vitro. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Defined Conjugation of Glycans to the Lysines of CRM197 Guided by their Reactivity Mapping

Systematic characterisation of the reactivity of the lysine moieties in CRM₁₉₇ towards N‐hydroxysuccinimide linkers bearing alkynes or azides is described. This involves two‐step conjugation of various glycans to CRM₁₉₇ by click chemistry in a well‐defined manner. By semiquantitative LC‐MS/MS analysis of proteolytic digests of the conjugates formed, the reactivity of lysine residues in the protein was mapped and ranked. Computational analysis of the solvent accessibility of each lysine residue (based on the CRM₁₉₇ crystal structure) established a correlation between reactivity and surface exposure. By this approach, conjugation involving lysine residues (normally a random process) can be controlled. It enables the preparation of lysine‐mediated glycoconjugates with improved batch‐to‐batch reproducibility, thereby producing neo‐glycoconjugates with more‐consistent biological activity.     

Visualization of PVDF nanofibers coated on filter paper using fluorescein silica nanoparticles

Fluorescein silica nanoparticles (NPs) were prepared using a silane compound bound between fluorescein‐N‐hydroxysuccinimide (NHS‐Fluorescein) and 3‐aminopropylorthosilicate by a sol–gel method. The fluorescein‐silica NPs were mixed with a poly(vinylidene fluoride) (PVDF) solution, and the solution loaded with the NPs was electrospun on a filter paper. Scanning electron microscopy and transmission electron microscopy images confirmed the encapsulation of the fluorescein silica NPs in the PVDF nanofibers. Laser scanning confocal microscopy (LSCM) images showed fluorescein silica NPs as dots, and photoluminescence (PL) images obtained using a fluoroanalyzer indicated the emission of uniform PL from filter papers coated with fluorescein‐silica‐NP‐encapsulated PVDF nanofibers. It was demonstrated that the fluorescein silica NPs enabled PVDF nanofibers coated on a filter paper to be easily visualized. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 45125.     

Selektiv S-geschützte Cysteinpeptide. Zur Synthese von Cysteinpeptiden unter Verwendung der S-Äthylmercapto-Schutzgruppe

Selectively S-Protected Cysteine Peptides. Synthesis of Cysteine Peptides Using the S-Ethylthio Protecting Group Studying the problems of the selective sulphur protection in cysteine peptides, a model heptapeptide from the sheep insulin A-chain was prepared by conventional and solid phase synthesis using the S-ethylthio and the S-diphenylmethyl group. The conventional synthesis of the heptapeptide N-tert.-butyloxycarbonyl-S-ethylthiocysteinyl-S-diphenylmethylcysteinyl-alanyl-glycyl-valyl-S-ethylthiocysteinyl-alanine 1 was carried out with the fragments N-tert.-butyloxycarbonyl-S-ethylthiocysteinyl-S-diphenylmethyleysteinyl-alanyl-glycine 2 and valyl-S-ethyl-thiocysteinyl-alanine 3 by means of the hydroxysuccinimide ester of 2 . Because of the small stability of S-ethylthio-protected cysteine peptides against alkali, 2 was synthesized without carbonyl protecting group by hydroxysuccinimide ester couplings from the carboxyterminal end, whereas 3 was obtained using the 2-p-toluenesulphonyl ethyl ester carboxyl protecting group, which can be saponified selectively at pH 10 preserving the S-protecting group. The S-ethylthio group exhibits only a small acid stability and was not completely stable during the deprotection of the N^α-Boc-group. Therefore neither 3 nor 1 could be obtained in a pure state by solid phase technique.     

Cu_3N薄膜制备及其性能研究

Cu3N薄膜的晶面取向、沉积速率、电学特性等性质除与制备方法有关外,还和制备工艺参数有很大关系。溅射法制备Cu3N薄膜工艺参数主要有,混合气体(N2+Ar)中氮气分压比r、基底温度T(℃)、溅射功率P(W)。为了研究Cu3N薄膜的性能与其制备工艺参数之间关系,本文采用反应射频磁控溅射法,在玻璃基底上成功制备了Cu3N薄膜,并研究了工艺参数对其晶面取向、膜厚、电学性能、沉积速率的影响。     

2-氯-5-甲基吡啶的合成方法

介绍了2-氯-5-甲基吡啶的四种类型的合成方法,包括以3-甲基吡啶-N-氧化物为原料的氯化法、2-氨基-5-甲基吡啶氯化法、环合氯化法、3-甲基吡啶直接氯化法等     

Polysaccharide‐based artificial extracellular matrix: Preparation and characterization of three‐dimensional,macroporous chitosan,and heparin composite scaffold

Scaffold‐guided tissue engineering based on synthetic and natural occurring polymers has gained many interests in recent year. In this study, the development of a chitosan‐heparin artificial extracellular matrix (AECM) is reported. Three‐dimensional, macroporous composite AECMs composed of heparin (Hep) and chitosan (Chito) were prepared by an interpolyelectrolyte complex/lyophilization method. The Chito‐Hep composite AECMs were, respectively, crosslinked with glutaraldehyde, as well as cocrosslinked with N,N‐(3‐dimethylaminopropyl)‐N′‐ethyl carbodiimide (EDC/NHS) and N‐hydroxysuccinimide (NHS). The crosslinking reactions were examined by FT‐IR analysis. In physiological buffer solution (PBS), the EDC/NHS‐crosslinked Chito‐Hep composite AECM showed a relative lower water retention ratio than its glutaraldehyde‐crosslinked counterparts. The EDC/NHS‐crosslinked Chito‐Hep composite AECMs showed excellent biocompatibility, according to the results of the in vitro cytotoxic test. This result suggested that the EDC/NHS‐crosslinked Chito‐Hep composite AECMs might be a potential biomaterial for scaffold‐guided tissue engineering applications. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

New conducting thermoplastic elastomers. I. Synthesis and chemical characterization

In the last 20 years, much interest has been focused on conducting polymers to find new materials to transfer from research to industry. However, in many cases, as for elastomers for which intrinsically conducting materials are unavailable, it is necessary to use conducting particles that are physically mixed with the polymeric matrix to give loaded rubbers. In this work we report the synthesis and the chemical characterization of an intrinsically conducting material with good mechanical and electrical conduction properties. To achieve such a global goal, we covalently linked, by an amidation reaction, the terminal NH₂ of Emeraldine (EB) and sulfonated Emeraldine (SPAN) to a free carboxylic group belonging to the repetitive unit of a functionalized segmented polyurethane. The reaction was carried out by activating such a carboxylic group with N,N′‐dicyclohexylcarbodiimide and N‐hydroxysuccinimide. The reaction yields and the chemical properties of the polymers were studied by proton and carbon‐13 nuclear magnetic resonance, ultraviolet, and Fourier transform infrared spectroscopy. The average numbers of EB or SPAN aromatic rings per polyether urethane acid (PEUA) repetitive unit, which cannot be assumed to be amidation degree because at this moment the molecular weights of the inserted EB and SPAN chains are unavailable, were 6 in case of the polymer obtained from the pristine Emeraldine and 1 for that obtained from the sulfonated Emeraldine. This result could be because SPAN was used in the acidic form, which depresses the nucleophilicity of the NH₂ group because of the presence of the sulfonic protons. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 83: 857–867, 2002     

Surface‐functionalized polyurethane nanoparticles for targeted cancer therapy

Polymer nanoparticles (nps) have gained growing interest as carriers for anticancer drugs as they can target tumour tissues by both passive and active pathways. While the passive targeting mechanisms mainly rely on the small size of the carriers, active targeting requires surface modifications of the polymer core in order to introduce specific functionalities to actively recognize cancer cells. The present work proposes an innovative method for the preparation of surface‐functionalized nps based on the use of biodegradable polyester‐ and polyester/ether‐urethanes (PURs) embedding amino functionalities. Two polyurethanes were prepared, one based on just poly(?‐caprolactone) diol (PCL‐PUR) and the other based on both PCL diol and poly(ethylene glycol) (PEG) (70/30 ratio, PCL‐PEG‐PUR). Nanoparticles of small size ranging between 150 and 200 nm and negative ζ potential (ranging from ?18 mV to ?27 mV) were obtained. Functional groups were exposed post nps preparation as confirmed by X‐ray photoelectron spectroscopy, ninhydrin assay and ¹H NMR, which evidenced a 24% tert‐butyloxycarbonyl cleavage for PCL‐PUR‐NH₂ nps and 29% for PCL‐PEG‐PUR‐NH₂ nps. The monoclonal antibody Herceptin (HER), which targets HER‐2 receptors, was coupled through ethyl(dimethylaminopropyl) carbodiimide/N‐hydroxysuccinimide (EDC/NHS) mediated chemistry. The optimal HER:NH₂ ratio was determined to be 1:16 for the PEG‐containing PUR and 1:8 for PCL‐PUR. HER‐nps maintained the intrinsic cytotoxicity of the antibody, as shown by the ca 50% decrease of HER‐2‐expressing HeLa cell viability. The results indicate that our protocol for surface functionalization of PUR nps, based on surface exposure of previously inserted functional groups followed by covalent coupling of biomolecules, is suitable for the preparation of nps for active recognition of target cells. © 2016 Society of Chemical Industry     

Synthesis of polylactide/poly(ethylene glycol) diblock copolymers with functional endgroups

Amphiphilic polylactide/poly(ethylene glycol) (PLA–PEG) diblock copolymers with functional groups at the PEG chain ends were synthesized by coupling PLA and PEG homopolymers using different coupling agents. PLA precursors with different endgroups were synthesized by ring‐opening polymerization of l ‐lactide in the presence of different initiators such as octanol, acetic acid or benzoic acid, or water, using non‐toxic zinc lactate as catalyst. The mechanism of the ring‐opening polymerization of lactide initiated by carboxyl groups was investigated and discussed in comparison with the literature. N,N'‐carbonyldiimidazole was used to couple the two hydroxyl groups of PLA and PEG, using 4‐dimethylaminopyridine (DMAP) as catalyst. Dicyclohexylcarbodiimide (DCC) and DMAP were adopted to couple the carboxyl group and the hydroxyl group of PLA and PEG, respectively, while DCC and N‐hydroxysuccinimide were used to connect PLA and PEG by coupling their carboxyl and amine groups. Comparison of different coupling routes shows that the DCC/DMAP one exhibits the highest efficiency. A common tumor targeting ligand, folic acid, was attached to PLA–PEG with hydroxyl endgroups using the DCC/DMAP route. The resulting PLA–PEG copolymers bearing folic acid present great interest for targeted delivery of anti‐cancer drugs. © 2012 Society of Chemical Industry