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Ti(OPr^i)4作为氧化剂直接氧化有机物尚属首例, ti(OPr^i)4很容易将苯偶姻氧化生成苯偶酰。室温下, 以THF作溶剂, 反应仅需10min。同样, Ti(OPr^i)4也能将氯、甲基和甲氧基取代的苯偶姻以及糠偶姻(Furoin)氧化生成相应的二酮。实验结果表明:Ti(OPr^i)4与苯偶姻体系的反应, 条件温和, 产率很高, 是一条实用、而有效的由苯偶姻制备苯偶酰的途径。 相似文献
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报道了盐酸三甲胺三氧化锆/硅胶载体试剂的制备方法及其对苯偶姻的氧化反应。该试剂制备简单,用于地苯偶姻的氧化,高收率地得到相应的苯偶酰在化合物,并且反应条件温和,产物易分离。 相似文献
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Fe2O3/Al2O3催化氧化苯偶姻制备苯偶酰 总被引:13,自引:1,他引:13
考察了几种常用载体负载金属氧化物催化分子氧氧化苯偶姻制备苯偶酰的性能 ,发现氧化铁、三氧化二铝催化活性较高,稳定性较好。以吡啶为溶剂,用483K下 活化的含铁14.8%的氧化铁/三氧化二铝作催化剂,当其用量为苯偶姻用量20% (质量分数),253K下反应1h,苯偶酰平均产率98.1%。用IR,MS,和^1H NMR光 谱对其结构进行了表征。 相似文献
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以绿色廉价的乙醇-水为溶剂,一锅法合成了金属萨伦(Salen)配体催化剂[M(Salen)](M=Co,Cu,Zn,Fe,Mn),完成了安息香氧化制备苯偶酰。 产物结构通过1H NMR、13C NMR、IR、HRMS及XRD等技术手段进行了表征。 通过正交设计实验考察了催化剂质量浓度、反应时间、溶剂、反应温度、KOH质量浓度等因素对反应的影响,获得了最优条件。 实验结果表明,以[Co(Salen)]作为催化剂(1.7×10-3 g/mL),80%(体积分数)乙醇作为溶剂,70 ℃,反应50 min,苯偶酰产率达到76.5%。催化剂循环使用5次,苯偶酰收率仍可达74.2%。 为绿色制备苯偶酰提供了一种新途径。 相似文献
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CrO3.CH3NH2.HCl/Al2O3的制备及其对苯偶姻体系的氧化反应 总被引:1,自引:0,他引:1
CrO3·CH3NH2·HCl/Al2O3的制备及其对苯偶姻体系的氧化反应张贵生*石启增陈密峰蔡昆(河南师范大学化学系新乡453002)关键词CrO3·CH3NH2·HCl/Al2O3,苯偶姻,苯偶酰,氧化1996-08-18收稿,1996-11-0... 相似文献
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安息香是合成许多类似物的中间体,苯环上可以带有不同的取代基,也可以改为含杂原子的芳核,因此对安息香缩合反应的研究很多。糠偶姻是合成有机金属试剂糠偶姻单肟和α-糠偶酰二肟的中间体,一般用乙醇-水为溶剂,以氰化钾(或钠)为催化剂,用糠醛经安息香缩合反应制成,产率可达37.5%。人们为了提高产率,曾经使用 相似文献
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在氯合5,10,15,20-四苯基卟吩合铁(III)[TPPFe(III)Cl]催化下, 带有不同取代基的亚碘酰苯和亚碘酰苯的衍生物作充氧化剂对环己烷进行了仿生单充氧化反应的研究.取代亚碘酰苯中对位取代基的电子效应和间位取代基的电子及立体效应对氧化产物环己醇的产率有良好线性相关性. 亚碘酰苯的衍生物苯亚碘酸二醋酐与苯亚碘酸单对甲苯磺酸酐对环己烷的充氧化能力和邻、间、对亚碘酰苯甲酸与邻亚碘酰苯甲酸酯相似, 环己醇产率接近零. 从而提出亚碘酰苯甲酸及邻亚碘酰苯甲酸酯存在分子内或分子间I(oh)oco成键结构的论点. 相似文献
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本文研究了各种Ti(Ⅳ)化合物:Ti(OR)_4(R=Et,~iPr,~nBu),TiCl_4,CP_2TiC_2,Cp_2Ti(OPh)_2对Meerwein-Ponndorf-Verley-Oppenauer反应的催化活性。试验表明Ti(O~iPr)_4对还原反应显示出极好的催化活性,还原苯甲醛,对氯苯甲醛,对硝基苯甲醛,对甲氧基苯甲醛,糠醛,巴豆醛的产率可达80%以上。Ti(OEt)_4对氧化反应有良好的催化活性,对正辛醇,2-辛醇,苯甲醇,环已醇,肉桂醇的氧化产率在69%以上。同时还考察了各种参数对反应的影响。 相似文献
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The accelerated growth of aquaculture has resulted in a series of harmful effects to human health. The widespread and unrestricted use of antibiotics in this industry, to prevent bacterial infections, leads to remaining amounts in the aquatic environment. This has resulted in the emergence of antibiotic-resistant bacteria in aquaculture environments, in the increase in antibiotic resistance in fish pathogens as well as in the transfer of these resistance determinants to human pathogens. Moreover, the use of large amounts of antibiotics may lead to the presence of residual antibiotics in fish tissue and fish products. Fluoroquinolones, tetracyclines, penicillins, sulphonamides and other antibiotics, exhibiting activity against both Gram-positive and Gram-negative bacteria, are widely used for the treatment and prevention of diseases in fish. An extended and comprehensive review on the recent analytical methodologies concerning antibiotic residues in fish reported in the literature is provided in the present article. Emphasis is given on sample preparation regarding isolation and purification, chromatographic conditions and method validation according to legislation. Results of published assays are comparatively presented and criticised. 相似文献
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P.N. Joshi N.K. Ramaswamy M.K. Raval T.S. Desai P.M. Nair U.C. Biswal 《Journal of photochemistry and photobiology. B, Biology》1993,20(2-3):197-202
Wheat seedlings, grown for 7 days in the light, were allowed to senesce in the light or dark, and the change in the photosystem II (PS II) photochemistry of chloroplasts isolated from the primary leaves of these seedlings was investigated. The decrease in oxygen evolution and the fast fluorescence results indicated that the impairment of PS II in the leaves of seedlings senescing in the light was different from that in the leaves of seedlings senescing in the dark. Thermoluminescence studies showed a structural modification in the QB protein of chloroplasts isolated from leaves senescing in the light and an alteration in the S state transition of chloroplasts isolated from leaves senescing in the dark. 相似文献
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辛厚文 《化学物理学报(中文版)》2000,13(4):388-405
化学体系中随机共振现象的特性、机理、本质和应用的研究是非常重要的前沿课题。综述中国科学技术大学非线性化学实验室,在化学体系随机共振现象的理论研究中,所取得的主要成果,并阐述化学体系随机共振现象研究中所提出来的若干重要问题:非均相化学体系中随机共振;化学体系中内信号随机共振;化学体系中多重随机共振;化学体系中随机共振的调制;化学体系中色噪声作用下的随机共振;化学体系中时空随机共振;耦合化学体系中随机共振;化学体系中双参量随机共振。 相似文献
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综述了壳聚糖、甲壳素在污水处理、电化学、原子吸收光谱、高效液相色谱、吸光光度法中的应用。引用文献28篇。 相似文献
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用原子吸收光谱法测定延边地区317名65~108岁老人头发中锌、铜、铁、锰、镁含量,观察不同民族、性别、年龄老人这些元素的差异。结果表明:1.朝鲜旗发锌低于汉族,满族发铜低于汉族、朝鲜族,汉族发镁高于朝鲜族、满族,发铁、发锰在汉、朝、满民族之间无区别。2.汉族、朝鲜族男发锌高于女性,汉族女性发铜高于男性,发铁、发锰、发镁在性别之间无区别。3、90岁组朝鲜族发锰、发镁低于65岁、76岁组,朝鲜族发锌、发铜、发铁在65~108岁之间无统计学意义。 相似文献
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Calibration methods for microdialysis sampling were studied in the muscle and adipose tissue of rats. Both the delivery method and the no-net-flux method were used to determine the extraction efficiency (EE) of acetaminophen and caffeine in both tissues. There was no concentration dependence of the EE either in vitro or in vivo for either acetaminophen or caffeine. The EEs determined by the delivery and no-net-flux methods were not different. However, the EEs of both caffeine and acetaminophen determined in vitro were significantly higher than those determined in the muscle and adipose. This indicates that mass transfer in the tissue is the rate-determining factor for the EE in vivo. The relative difference between the EE in vitro and the EE in the muscle was smaller than the difference between the EE in vitro and the EE in the adipose. In addition, the EE in the muscle decreased more than the EE in the adipose after the animal was euthanized. This indicated that exchange between the extracellular fluid and plasma is the rate-determining step in mass transport relative to microdialysis sampling. This has a more significant effect on the EE in the muscle than the EE in the adipose. Both the delivery and no-net-flux methods can be used to calibrate microdialysis probes in the muscle and adipose. 相似文献
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Peter N. Taylor Andrew P. Wylie Juhani Huuskonen Harry L. Anderson 《Angewandte Chemie (International ed. in English)》1998,37(7):986-989
Despite their larger separation , the porphyrin groups in 1 are more strongly conjugated than in analogous compounds in which butadiyne is the bridging unit. This stronger electronic coupling in 1 results in a bathochromic shift in its absorption and emission spectra. 相似文献
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Hiroshi Hasegawa 《应用有机金属化学》1997,11(4):305-311
Seasonal changes in the distribution of arsenic species were observed in a dredged area in the southern basin of Lake Biwa, Japan. The concentrations of dimethylarsenic acid [DMAA(V)] became comparable with those of inorganic forms during a stratification period. DMAA(V) increased not only in the photic zone but also in the hypolimnion. In the photic zone, an increase in DMAA(V) was observed with the yearly maximum of water temperature. In the hypolimnion, the seasonal changes in methylarsenicals differed from those in surface waters. DMAA(V) maxima appeared seasonally under sub-anoxic conditions and developed regionally at the redox boundary and above the sediment surface. The DMAA(V) concentrations increased in the initial period of oxygen depletion and just after the disappearance of anoxia, while they diminished in the anoxic hypolimnion by midsummer. The seasonal behavior of trivalent methylarsenicals, which are readily oxidized in oxic environments, was similar to that of DMAA(V). The total arsenic concentration in the surface layer rose to a maximum in late summer. Methylarsenicals did not increase in such a way that the total arsenic concentration increased during summer. © 1997 by John Wiley & Sons, Ltd. 相似文献
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C. Albelda Y. Pico J. C. Molto G. Font J. Mañtes 《International journal of environmental analytical chemistry》2013,93(1-4):315-326
Abstract The accumulation, persistence and fate of systemic pesticide aldicarb was melencholy evaluated in orange crops. The concentration of this pesticide and its two toxic metabolites, aldicarb sulfoxide and aldicarb sulfone was determined in leaves, rind and pulp of three orange varieties (Satsuma, Navelina and Clemetina de Nules) and in the top soil of the orange groves. The groves were located in two different places in the Valencia Community (Spain). The analysis showed that the aldicarb concentration was lower than those of aldicarb sulfoxide and aldicarb sulfone. In all cases, the residues persisted at least 160 days in vegetable samples and between 157 and 227 days in soil samples. Residue concentrations measured in the soil samples were highly variable but a relation with the organic matter content can be observed. The residue levels found in vegetal products were higher in leaves than in rind, and in rind than in pulp. The maximum residue values were obtained between 47 and 70 days after the application. One hundred days after treatment (Security period) the residue levels of total fruit were lower than the maximum residue level of 0.2 mg/kg established by law. 相似文献