N-己基咔唑-3-硼酸频那醇酯的合成与表征

以3-溴咔唑为初始原料,经Miyaura Borylation反应、亲电取代反应合成了有机发光材料中间体N-己基咔唑-3-硼酸频那醇酯,通过NMR表征了化合物的结构,高效液相色谱检测目标化合物含量大于99.5%,合成方法简单,适用于工业化生产。     

新手性N-苄氧甲酰基氨基酸芳基酯的微波合成和生物活性研究

用N,N'-二环己基碳二亚胺作脱水剂,在微波辐射条件下,N-苄氧甲酰基氨基酸和酚缩合反应生成了一系列新的N-苄氧甲酰基氨基酸芳基酯,缩短了反应时间。目标化合物的结构经1HNMR,13CNMR,IR和MS等进行了表征。对所合成的目标化合物进行了初步的生物活性测试,结果表明目标化合物具有一定的杀虫活性和杀菌活性,杀菌活性高于杀虫活性。     

新型含吡啶杂环菊酯类化合物的合成及生物活性

为了寻找新的活性化合物,根据活性亚结构拼接原理,以四丁基溴化铵为相转移催化剂,以3,5-二氯-6取代胺基吡啶杂环的酚钠盐和菊酰氯为原料,在二氯甲烷-水混合体系中合成了一系列新型含吡啶杂环菊酯类化合物。其结构均经1HNMR、13CNMR、IR和MS等分析方法确证。初步生物活性测试结果表明,化合物4e和4f具有有效的杀菌活性,在500mg/L时对黄瓜白粉病菌的抑制率均为100%,对黄瓜炭疽病菌的抑制率分别为60%、56.8%。     

Indirect Method for Simultaneous Determinations of 3-Chloro-1,2-Propanediol Fatty Acid Esters and Glycidyl Fatty Acid Esters

Recent concerns about potential health risks associated with 3-chloro-1,2-propanediol fatty acid esters (3-MCPD esters) and glycidyl fatty acid esters (GEs) in refined vegetable oils and fats have led to development of various methods for quantitative determinations of these compounds. Among them, indirect methods, which determine total amount of 3-MCPD and glycidol after hydrolysis of the esters, have an advantage over direct methods, which require a reference standard for each of the many possible species of fatty acid esters to be quantified. The existing indirect methods, however, may yield unreliable results or require long hours of alkaline methanolysis. To overcome these shortcomings, the objective of this study was to develop a reliable and rapid indirect method for simultaneous determinations of 3-MCPD esters and GEs. By using Candida rugosa lipase and sodium bromide for a hydrolysis/bromination step, 3-MCPD esters and GEs were transformed within 30 min to 3-MCPD and 3-bromo-1,2-propanediol (3-MBPD), respectively, without interconversion. Gas chromatography–mass spectrometry (GC–MS) analysis of 3-MCPD and 3-MBPD derivatized with phenylboronic acid showed 89–108 % recovery of 3-MCPD-diesters, -monoesters, and GEs from various oils and fats spiked at 2 and 20 mg/kg. The method should be useful for routine analysis of 3-MCPD esters and GEs.     

富马酸烷·3-PG酯的合成研究

研究 5种具有良好的抗氧化和抗菌活性的新型化合物———富马酸甲 (乙、丙、丁、戊 )·3 PG酯的合成工艺条件并揭示了其规律。发现富马酸单酯单酰氯与没食子酸丙酯 (PG)的理想反应条件为 :在c(PG) =5 7 0 1mol/L的吡啶溶液中 ,吡啶正常回流温度下 ,分别缓慢滴加富马酸单甲 (乙、丙、丁、戊 )酯单酰氯 ,反应 4 0～ 6 0min ,可获得产率为 75 6 % (78 3%、83 8%、83 3%、76 5 % )的富马酸甲 (乙、丙、丁、戊 )·3 PG酯。随烷基碳链的增长 ,马来酸酐与醇的物质的量比减小 ,反应温度升高和反应时间延长     

三价铬电镀装饰铬新工艺

开发了Trich-6771氯化物体系三价铬电镀装饰铬新工艺。在10A/dm2的电流密度下,沉积速率达到0.2μm/min,镀层厚度小于0.5μm。中性盐雾试验168h,乙酸盐雾试验96h,铜加速乙酸盐雾试验48h,镀层无明显变化。恒定湿热试验360h,镀层不长霉点。人造汗液测试和抗化学污染测试满足行业要求。     

卤代芳烃和苯硼酸的Suzuki偶联反应研究进展

Suzuki偶联反应是形成C-C键的有效方法之一,在天然产物合成和药物中间体合成中发挥着重要作用,近年来一直是有机化学和催化化学的研究热点.本文综述了最近几年来Suzuki偶联反应及其在有机合成中的应用研究进展,叙述了Suzuki偶联的原理,对以Pd、Ni、Cu及其它催化剂在Suzuki偶联反应中的应用进行了重点论述,...     

乳酸(酯)脱水制丙烯酸(酯)

丙烯酸是一种重要的有机合成原料及合成树脂单体,目前,生产丙烯酸的主要原料均来源于石化产品,但是石油资源越来越短缺,因此,开发经济可行地利用生物质资源制备丙烯酸是生成丙烯酸的重要研究方向之一。对近年来用乳酸脱水制备丙烯酸的研究工作进行了综述,重点介绍几种较有前景的由乳酸(酯)通过化学法或生物法制取丙烯酸的研究情况。     

富马酸烷·3-PG酯合成路线的设计

报道了富马酸烷·3 PG酯合成路线的设计思路 :以顺丁烯二酸酐为起始原料 ,与甲、乙、丙、丁、戊醇发生酯化反应制得五种马来酸单酯 ,马来酸单酯异构化为相应的富马酸单酯 ,后者与亚硫酰氯作用得到五种富马酸单酯单酰氯 ,用制得的富马酸单酯单酰氯酰化没食子酸丙酯 (PG)分子中的 3 羟基制得五种具有良好的抗氧化和抗菌活性的新型化合物———富马酸甲 (乙、丙、丁、戊 )·3 PG酯。     

C1-对称性手性二胺席夫碱金属配合物的研究进展

就近年来国内外对具有C1-对称性的手性二胺席夫碱(1R,2R)-N,N’-3,5-双取代水杨醛-1,2-环己二胺及其衍生物的金属配合物研究进展作一简要介绍,重点评述了这些配合物的合成方法以及它们作为手性催化剂在不对称合成中的应用。     

Utilization of Macroporous Polymer Containing Phenylboronic Acid Groups in the solid- phase synthesis

Ethylene glycol (4-vinylphenyl-)-boronate ( 2 ) was copolymerized with technical divinylbenzene to highly crosslinked macroporous polymer ( P2 ). On treatment of P2 with methanol/water, 75% of the polymer-bound ethylene glycol could be split-off, under formation of the desired polymer ( P1 ) with free phenylboronic acid groups. The utility of P1 in the solid-phase synthesis, for instance its conversion to polymer-supported phenol, and as polymer-supported protecting group for diols was investigated.     

异戊烯酸酯合成新法

以异戊烯酸和甲醇等醇类为原料,在三氯氧磷催化下一步合成相应的酯类。在酸醇物质的量比为1∶3时,三氯氧磷用量为20mL,反应4～5h,异戊烯酸甲酯、乙酯和丁酯的收率分别为86.2%、90.5%和80.3%。     

Infrared Studies on Isomeric Octadecadienoic Acid Esters

Glycerol esters of isomeric octadecadienoic acids prepared from dehydrated castor and safflower oils and several commercially available isomerized safflower oils were blended with oils of known compositions and analysed by standard infrared methods for cis- and trans-isomer content in both isolated and conjugated dienes. The agreement between the analytical data for the known and unknown mixtures was very good. For conjugated systems the absorptivities agreed with literature reports. Linoleic acid having the isolated cis-cis-structure was derived from naturally occurring oils and converted to the conjugated cis-trans-isomer by the alkali method. Esterification of the latter with glycerol at 190° to 220° C showed no appreciable change in isomeric structure. The conjugated trans-trans oils were prepared from the cis-trans isomer with iodine. The isolated trans-trans oil was obtained by treatment of safflower oil with selenium or nitrous acid.     

Topochemical Photodimerization of 4-(3-Oxo-3-phenyl-l-propenyl)benzoic Acid and Its Esters

The photodimerization behaviors of 4-(3-oxo-3-phenyl-1-propenyl)benzoic acid (1) and its esters (2–7) in the crystalline state are investigated. These crystals, except that of the phenyl ester (7), dimerize photochemically to yield the corresponding cyclobutane derivatives in a typical topochemical fashion. Head-to-head type cyclobutane derivatives are obtained from crystals of the acid and ethyl ester (1 and 3), whereas head-to-tail type derivatives are formed from the other ester crystals (2, 4, 5, and 6). The temperature dependences of these reaction behaviors and the configurations of the photoproducts are correlated with the molecular arrangement in the reactant crystals. Reversible or irreversible behavior of as-formed dimer crystals, derived from 2 or 4 crystals, is interpreted in terms of accumulated strain energy in the course of the topochemical process.     

糠酸酯的合成及香气研究

糠酸酯是一类重要的香味物质。为此以酰氯酯化法合成了一系列相应的酯类 ,并对酯类香气进行了感官评定 ,找出了其香气衍变的规律     

Crystallization Behavior of Fatty Acid Methyl Esters

Biodiesel from most agricultural feedstocks has flow properties that are prone to startup and operability problems during cold weather. Biodiesel from soybean oil is generally a mixture of long-chain fatty acid alkyl esters composed of 0.15–0.20 mass fraction saturated esters (melting point [MP] ≫ 0 °C) mixed with unsaturated esters (MP < 0 °C). This work investigates the crystallization properties of two saturated fatty acid methyl esters (FAME) commonly found in biodiesel from soybean oil. Differential scanning calorimetry (DSC) heating and cooling scans of methyl palmitate (MeC16), methyl stearate (MeC18) and methyl oleate (MeC18:1) in pure form were analyzed. Crystallization behavior in ternary FAME mixtures was inferred by the application of thermodynamic models based on ideal solution and freezing-point depression theories. Activity coefficients for MeC16 and MeC18 in MeC18:1 solvent were determined by analyzing DSC cooling curves for binary FAME mixtures. Eutectic points were predicted by both models. Crystallization onset temperatures inferred from freezing point depression theory were more accurate than those for ideal solutions with respect to a direct DSC cooling curve analysis of corresponding ternary mixtures. This work shows that the crystallization onset temperature (cloud point) of biodiesel may be predicted by freezing-point depression theory if the activity coefficients of the component FAME are known. The use of trade, firm, or corporation names in this publication is for the information and convenience of the reader. Such use does not constitute an official endorsement or approval by USDA or ARS of any product or service to the exclusion of others that may be suitable.     

乳酸及其低碳醇酯脱水合成丙烯酸（酯）的催化剂研究进展

丙烯酸及其酯应用广泛,全球需求量日益增加。目前,丙烯酸的制备主要靠丙烯部分氧化法,对不可再生资源石油高度依赖,而石油资源日渐短缺与丙烯酸需求快速增长产生矛盾不可避免。寻求一条可持续的绿色发展路线合成丙烯酸及其酯迫在眉睫,乳酸及其低碳醇脱水法就是丙烯酸及其酯制备的理想方法。文章对乳酸及其低碳醇酯脱水制备丙烯酸及其酯的催化剂及工艺条件进行了较为系统的总结,特别是对近十年的研究进展的总结。以二氧化硅负载的磷酸盐、硫酸盐催化剂研究较多,活性较高;以改性后的分子筛譬如Y型分子筛具有非常高的反应活性和丙烯酸及其酯的选择性。另外,锂皂石、膨润土的良好催化性能也值得关注。     

食品乳化剂柠檬酸甘油单,二酸酯的合成

采用以乙酸为溶剂,柠檬酸和单甘酯进行酯化反应合成了质量指标均符合ＦＡＯ／ＷＨＯ标准的柠檬酸甘油单,二酸酯,确定了合成的最佳工艺条件,并以此为原料配制了两种在常温下呈液态的复合型搞氧剂。试验结果表明,其抗氧化效果超过了国外同类产品,在油脂及含油食品中具有广泛应用价值。