微波法研制碱土金属氧化物负载型MCM-48碱性介孔材料

以立方相介孔分子筛MCM-48为载体,用微波辐射分散MgO或CaO和醋酸镁溶液浸渍等方法研制碱性介孔材料。MCM-48能经受微波辐射,负载碱性客体之后也保持介相结构。异丙醇分解探针反应表明:载体本身没有碱催化活性,而碱性MCM-48介孔材料的活性随温度升高而提高。本文还对介孔材料在微波分散和碱性催化方面的特点进行分析。     

微波辐射-酶耦合催化(MIECC)反应

将微波辐射用于非水相酶催化可以获得很多有别于常规加热下的反应结果.本文讨论了微波的非热效应在酶促反应中的表现,探讨了微波辐射对酶的结构、构象、活性及酶催化反应动力学的影响,以及微波辐射-酶耦合催化对反应的对映选择性、底物专一性、前手性选择性和区域选择性的影响.在大多数场合,适当的微波辐射不会损伤酶活而且可以提高反应速率,而对酶特异性的影响则不一而论.     

掺铁纳米TiO_2的制备及其光催化性能

以TiC l4为原料,采用微波加热与常规加热2步合成法制备掺铁纳米TiO2。用X射线粉末衍射(XRD)、透射电镜(TEM)、紫外可见吸收光谱(UV-V is)、光电子能谱(XPS)等测试技术对其进行了表征。结果表明,所制得的掺铁纳米TiO2是以锐钛矿为主相的混晶,平均粒径约为10 nm,适量Fe3+的掺杂能促进金红石相变,抑制锐钛矿晶粒的生长,使Ti2p电子结合能升高0.3 eV,并使TiO2吸光能力增强,带边吸收向可见光区移动。在UVA段(320~400 nm)光照下,通过对维生素VB12的光催化降解,发现掺入摩尔分数为0.5%的Fe3+的纳米TiO2能明显提高其光催化活性,使维生素B12的降解速率提高2.3倍。     

Preparation and Properties of Urease Immobilized onto Glutaraldehyde Cross-linked Chitosan Beads

Urease was immobilized onto the glutaraldehyde cross-linked chitosan beads that were prepared under microwave irradiation. The activity and the yield of activity of immobilized urease was 10.83 U/g B and 47.7%, respectively. The conditions of urease immobilization were optimized. The properties of the immobilized urease were investigated and compared with that of the free enzyme.     

Polyfunctional pyrazoles. 4. Synthesis of 3-[3-aryl-1-(2-ethoxycarbonyl)-4-pyrazolyl]acrylic and-propionic acids

3-(3-Aryl-4-formyl-1-pyrazolyl)propionic acids are converted by Knoevenagel condensation under conditions of microwave activation into 3-[3-aryl-1-(2-ethoxycarbonyl)-4-pyrazolyl]acrylic acids. Reduction of the latter with hydrazine hydrate in the presence of Raney nickel gives 3-[3-aryl-1-(2-ethoxycarbonyl)-4-pyrazolyl]propionic acids. __________ Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 5, pp. 686–690, May, 2006.     

Synthesis and Crystal Structure of 3,7,7-Trimethyl- 1-phenyl-4-（3-nitrophenyl）- 4,5,6,7,8,9-hexahydro-1H-pyrazolo [3,4-b]quinoline-5（6H）-one

The title compound (C25H24N4O3) has been prepared by the cyclocondensation of 5-amino-3-methyl-l-phenypyrazol, m-nitrobenaldehyde and dimedone in glycol under microwave irradiation without catalyst. The crystal structure was determined by single-crystal X-ray diffraction to be orthorhombic, space group Pbca with a=16.3331(10), b=13.8329(9), c=19.4163(12) A, V= 4386.8(5)A3, Z=8, Dc=1.298g/cm^3,μ=0.087 mm^-1, F(000)=1808, Mr=428.48, the final R=0.0519 and wR=0.1019. X-ray analysis revealed that the pyridine ring is of boat conformation and the six-membered ring fused with it adopts twist boat conformation.     

Microscale sample deposition onto hydrophobic target plates for trace level detection of neuropeptides in brain tissue by MALDI-MS

A sample preparation method that combines a modified target plate with a nanoscale reversed-phase column (nanocolumn) was developed for detection of neuropeptides by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS). A gold-coated MALDI plate was modified with an octadecanethiol (ODT) self-assembled monolayer to create a hydrophobic surface that could concentrate peptide samples into a approximately 200-500-microm diameter spot. The spot sizes generated were comparable to those obtained for a substrate patterned with 200-microm hydrophilic spots on a hydrophobic substrate. The sample spots on the ODT-coated plate were 100-fold smaller than those formed on an unmodified gold plate with a 1-microl sample and generated 10 to 50 times higher mass sensitivity for peptide standards by MALDI-TOF MS. When the sample was deposited on an ODT-modified plate from a nanocolumn, the detection limit for peptides was as low as 20 pM for 5-microl samples corresponding to 80 amol deposited. This technique was used to analyze extracts of microwave-fixed tissue from rat brain striatum. Ninety-eight putative peptides were detected including several that had masses matching neuropeptides expected in this brain region such as substance P, rimorphin, and neurotensin. Twenty-three peptides had masses that matched peaks detected by capillary liquid chromatography with electrospray ionization MS.     

液相微波介电加热法制备纳米粒子的研究进展

随着纳米科技的飞速发展,合成纳米材料的新方法层出不穷。在这些新方法当中,液相微波介电加热法近年来得到了飞速的发展,引起了科学界越来越多的关注。本文介绍了近年来液相微波介电加热法制备纳米粒子的一些研究进展,主要是该方法在制备金属、过渡金属氧化物和金属硫族化合物纳米粒子中的应用,并且对该领域未来的发展作了一些展望。     

Rapid synthesis of α-ketoamides using microwave irradiation-simultaneous cooling method

Microwave-assisted acyl chloride-isonitrile condensation and CaCO₃-mediated hydrolysis constitute a one-pot, 2-minute process to prepare α-ketoamides.     

2-[3-(Trifluoromethyl)phenyl]furo[3,2-b]pyrroles: synthesis and reactions

The synthesis and reactions of methyl 2-[3-(trifluoromethyl)phenyl]-4H-furo[3,2-b]pyrrole-5-carboxylate (1a) are described. Upon reaction with methyl iodide, benzyl chloride, or acetic anhydride, this compound gave N-substituted products 1b-d. By hydrolysis of compounds 1a-c, the corresponding acids 2a-c were formed, or by reaction with hydrazine-hydrate, the corresponding carbohydrazides 3a-c were formed. By heating 2-[3-(trifluoromethyl)phenly]-4H-furo[3,2-b]pyrrole-5-carboxylic acid (2a) in acetic anhydride, 4-acetyl-2-[3-(trifluoromethyl)phenyl]furo[3,2-b]pyrrole (4) was formed. By hydrolysis of 4, 2-[3-(trifluoromethyl)phenyl]-4H-furo[3,2-b]pyrrole (5a) was formed, and reactions with methyl iodide or benzyl chloride gave N-substituted products 5b-c. The reaction of 4 with dimethyl butynedioate gave substituted benzo[b]furan 6. Compound 3a reacted with triethyl orthoesters giving 7a-c, which afforded with phosphorus (V) sulphide the corresponding thiones 8a-c. The thiones 8a-c reacted with hydrazine hydrate to form hydrazine derivatives 9a-c. The reaction of triethyl orthoformiate with compounds 9a-c led to furo[2′,3′: 4,5]pyrrolo[1,2-d][1,2,4]triazolo[3,4-f][1,2,4]triazines 10a-c. Hydrazones 11a-c were formed from 3a-c and 5-[3-(trifluoromethyl)phenyl]furan-2-carboxaldehyde. The effect of microwave irradiation on some condensation reactions was compared with “classical” conditions. The results showed that microwave irradiation shortens the reaction time while affording comparable yields.