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以磺酸功能化咪唑离子液体为催化剂,以3-羟基丙酸甲酯为原料,采用自身酯交换法合成了具有生物可降解性能的聚羟基脂肪酸酯.系统考察了离子液体种类、反应温度以及聚合反应时间对反应性能的影响,同时采用红外、核磁、热分析等手段对产物进行表征.研究结果表明:阴离子为CF3SO-3的磺酸功能化离子液体在120℃的低温下催化聚合反应所得聚酯Mw可达10 159,收率82.1%;通过水洗方法可有效去除产物中的离子液体催化剂,从而避免催化剂污染产物. 相似文献
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(S)-2-乙氧基-3-(4-羟基苯基)丙酸乙酯的合成;二乙氧基乙酸乙酯;Horner Wadswordth Emmons反应;催化氢化;化学拆分;(S) 乙氧基(羟基苯基) 相似文献
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标题化合物C19H23O4Cl(4)是由邻氯苯甲醛(1)与5,5-二甲基-1,3-环己二酮(2)、2,2-二甲基-1,3-二氧六环-4,6-二酮(3)在乙醇中反应而得。结构通过单晶X-射线衍射分析确定,其晶体属于单斜晶系,空间群晶体结构用直接法解出,使用全矩阵最小二乘法对原子参数进行修正,最后的偏离因子R=0.034,Rw=0.042。在晶体结构中存在一个共轭的烯醇结构。单晶X-射线分析表明;平面1(C(1)~C(6)、Cl)和平面2(C(8)~C(10)、C(12)、C(13))之间的两面角为97.11°,原子C(7)呈变形的四面体构型。 相似文献
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3-氨基-5,7-二羟基-4-甲基香豆素(4)是一种新的重要有机合成中间体,可用于多种潜在生物活性物质的合成。本文将间苯三酚与2-乙酰氨基乙酰乙酸乙酯(2)在BF3.Et2O的催化作用下,经串联的Pechmann缩合反应和脱乙酰基反应一锅合成4。化合物2由乙酰乙酸乙酯经成肟、还原、酰化反应制得。中间体和目标物的结构均经1H NMR、13C NMR、MS表征。该方法具有原料廉价易得、步骤短、操作简便易控、反应条件温和、收率高的优点。 相似文献
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PVA-GA-CS/PVA-Fe-SA bipolar membrane was prepared by a paste method. PVA-sodium alginate (SA) and PVA-chitosan (CS) were cross-linked by FeCl3 and glutaraldehyde (GA), respectively. The charge densities of PVA-CS and PVA-SA solutions were determined by the colloid titration. The swelling level of bipolar membrane was in the range of 25–85%, meanwhile the permeability and the ion-exchange capacity as well as co-ion transport properties was investigated. FTIR was applied to analyze the functional groups of the bipolar membrane. Furthermore, SEM photographs of the BPM cross-section illustrated a structure that consists of an anion layer (PVA-GA-CS) and a cation layer (PVA-Fe-SA). TG analysis of PVA-GA-CS/PVA-Fe-SA bipolar membranes exhibited a good thermal stability. PVA-GA-CS/PVA-Fe-SA bipolar membranes were used as the separator in the electrolysis cell for electro-generation of 2,2-dimethyl-3-hydroxypropionic acid. The average current efficiency was 52.2%, and the highest current efficiency reached 68.9%. 相似文献
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以聚丙烯腈为原料,首先通过部分腈基的[3+2]合环反应转化为聚(乙烯基四唑-co-丙烯腈)[Poly(VT-co-AN)],再通过碱性水解反应将剩余的腈基转化为羧基,合成出聚(乙烯基四唑-co-丙烯酸)[Poly(VT-co-AA)]。 采用傅里叶红外变换光谱仪(FT-IR)、核磁共振碳谱仪(13C NMR)、酸碱滴定等方法对Poly(VT-co-AN)和[Poly(VT-co-AA)的结构进行了表征,结果表明,Poly(VT-co-AN)的分子链中含有腈基、四唑基团和部分羧基,四唑基团的含量为68.6%,与酸碱滴定法测定的四唑基团的含量相近,[Poly(VT-co-AA)中含有四唑基团和羧基,不含有腈基,酸值高于Poly(VT-co-AN),四唑基团的含量为67.6%,与叠氮化钠与聚丙烯腈的摩尔比相近。 热失重分析结果显示[Poly(VT-co-AA)的热分解速率加快,在270~285 ℃的温度区间内分解完全。 相似文献
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V. A. Mamedov V. N. Valeeva L. A. Antokhina A. V. Chernova R. R. Shagidullin G. M. Doroshkina I. A. Nuretdinov 《Russian Chemical Bulletin》1994,43(8):1368-1372
Esters and amides of 2,2-dichloro-3-(2-furyl)-3-hydroxypropionic acid were prepared by the reaction of furfural with dichloroacetic acid derivatives under the conditions of the Darzens condensation. The structures of the reaction products were confirmed by their1H NMR and IR spectra and chemical transformations.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 1444–1448, August, 1994. 相似文献
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Dina A.S. Marques Susana Jarmelo Cristina M.S. G. Baptista M.H. Gil 《Macromolecular Symposia》2010,296(1):63-71
The step-growth polymerization of L-lactic acid in solution was studied in this work. In order to attain a polymer with high molecular weight, the water formed during the polymerization must be continuously removed. The use of organic solvents with high boiling point, drying agents and reduced pressure led to poly(lactic acid) (PLA) with high molecular weight, directly from the monomer. Tin (II) chloride dihydrate, SnCl2.2H2O, was the best of the catalysts tested as it allowed achieving PLA with a molecular weight close to 80 000 g.mol−1. However, the stereoregurarity control is a severe problem in PLA synthesis by step-growth due to transesterification reactions, which lead to an inversion of the conformation and a decrease of the optical purity of the polymer. Specific rotation measurements were used in this work and showed to be a powerful technique to evaluate the racemization extent. The thermal stability of the PLA samples was evaluated by DSC which exhibits a thermal behaviour similar to the commercial Polylactide. 相似文献
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Portilla-Arias JA García-Alvarez M de Ilarduya AM Holler E Galbis JA Muñoz-Guerra S 《Macromolecular bioscience》2008,8(6):540-550
Methyl esters of microbial poly(beta,L-malic acid) for conversion degrees of 25, 50, 75, and 100% were prepared by treatment of the polyacid with diazomethane. Esterification proceeded with retention of the molecular weight of the parent polyacid and the copolymers displayed a blocky microstructure consisting of short segments of malic and methyl malate sequences. The thermal stability of the copolyesters was lower than those of the parent homopolymers and all of them were fairly crystalline with melting temperatures within the range of 170-175 degrees C. They were degraded rapidly by water, the hydrolysis rate being highly dependent on the methylation degree. Microspheres with mean-average diameters in the range of 1-20 microm were prepared from the 100% methylated product by the emulsion-evaporation solvent method. Encapsulation of erythromycin was efficiently performed in these microparticles and its releasing upon incubation in simulated physiological medium was evaluated for different drug loads. Drug delivery was observed to occur by a releasing mechanism largely determined by the hydrodegradation of the host polymer and independent of the amount of loaded drug. 相似文献
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A synthetic route to higher molecular weight processable polyesters with bisphenol A terephthalate/isophthalate moieties and lactide moieties which are of potential interest for tissue engineering is described. The combination of aliphatic and aromatic moieties is a promising concept for processable polyesters with potential sites for physiological degradation and improved mechanical properties. The molecular structure of the copolyesters prepared by melt condensation via an acid chloride route and incorporation of the lactide moieties by transesterification of an oligo dl -lactide was confirmed by infrared, 1H and 13C nuclear magnetic resonance spectroscopy as well as gel permeation chromatography. The thermal and mechanical properties of copolyesters with different amounts of lactide moieties are reported and correlated with their composition. The reaction mechanism by transesterification was proved by a model reaction with a physical blend of the components and the hydrolytical behavior of the copolyesters under physiological conditions has been investigated. © 1997 John Wiley & Sons, Ltd. 相似文献
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Synthesis and reactivity of 3-(trichlorogermyl)propanoic acid and 3-(triphenylgermyl) propanoic acid
3-(Trichlorogermyl)propanoic acid (la) reacts with phenylmagnesium bromide in malar ratio 1:4 to give 3-(triphenylgermyl)propanoic acid (2a).In the compounds la and 2a theβ-carboxylic functional group shows some unusual properties when they react with excess of phenylmagnesium bromide.The compound la reacts with phenylmagnesium bromide in molar ratio 1:5 to give phenyl 2-(triphenylgermyl)ethylketone (3a) and in molar ratio 1:6 to give l,l-diphenyl-3-(triphenylgermyl)propanol (4a).The compound 2a reacts with phenylmagnesium bromide in molar ratio 1:2 to give 3a and in molar ratio 1:3 to give 4a also.Dehydration of the compound 4a with dilute hydrochloric acid seems especially easy.Moreover,the compound la reacted with phenylmagnsium bromide in molar ratio 1:6,then the mixture was treated with dilute hydrochloric acid to give 1,1-diphenyl-3-(triphenylgermyl)-1-propene (5a) in one pot reaction.Alkyl Ge-C bond in the compound 5a can be cleaved selectively by lithium aluminium hydride ( LiAlH4) in good yiel 相似文献
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Julien Babinot Estelle Renard Valrie Langlois 《Macromolecular rapid communications》2010,31(7):619-624
A new synthesis of amphiphilic biodegradable copolymers consisting of hydrophobic poly(3‐hydroxyalkanoate) (PHA) backbone and hydrophilic poly(ethylene glycol) (PEG) units as side chains is described. Poly[(3‐hydroxyoctanoate)‐co‐(3‐hydroxyundecenoate)] (PHOU) was first methanolyzed and its unsaturated side chains were quantitatively oxidized to carboxylic acid. Esterification with propargyl alcohol led to an alkyne‐containing “clickable” PHA in 71% conversion. Its reactivity was successfully demonstrated by grafting azide‐terminated PEG chains of 550 and 5 000 g · mol−1, respectively. All products were fully characterized using GPC, 1H, and COSY NMR.