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151.
This Letter describes the amination of 3-bromoisoxazoles by a nucleophilic aromatic substitution reaction. We have found 3-bromoisoxazoles to be inert to substitution under thermal conditions, however, the employment of phosphazene bases under microwave irradiation facilitates the amination process and allows the corresponding 3-aminoisoxazoles to be isolated in moderate yield. 相似文献
152.
153.
Norimah Yusof Asnah Hassan M.N. Firdaus Abd Rahman Suzina A. Hamid 《Radiation Physics and Chemistry》2007,76(11-12):1756-1759
Most of the tissue banks in the Asia Pacific region have been using ionising radiation at 25 kGy to sterilise human tissues for save clinical usage. Under tissue banking quality system, any dose employed for sterilisation has to be validated and the validation exercise has to be a part of quality document. Tissue grafts, unlike medical items, are not produced in large number per each processing batch and tissues relatively have a different microbial population. A Code of Practice established by the International Atomic Energy Agency (IAEA) in 2004 offers several validation methods using smaller number of samples compared to ISO 11137 (1995), which is meant for medical products. The methods emphasise on bioburden determination, followed by sterility test on samples after they were exposed to verification dose for attaining of sterility assurance level (SAL) of 10−1. This paper describes our experience in using the IAEA Code of Practice in conducting the validation exercise for substantiating 25 kGy as sterilisation dose for both air-dried amnion and those preserved in 99% glycerol. 相似文献
154.
JinXianWANG XiaoNingSHI KeHuWANG XiuQinMEN 《中国化学快报》2004,15(3):284-285
An efficient and convenient synthesis of 3, 5, 7-triaryl-4H-1, 2-diazepine from 2, 4,6-triarylpyrylium salts and hydrazine in water under microwave irradiation is reported. The same reaction can be conducted using 2, 4, 6-triarylthiopyrylium salts and hydrazine. 相似文献
155.
桥联双(甲巯咪唑)化合物的合成和配位性能 总被引:3,自引:0,他引:3
研究了桥联双(甲巯咪唑)化合物(Ⅰ_a—Ⅳ_a、Ⅰ_b)的合成和配位性能。UV谱显示Ⅰ_a—Ⅳ_a与UO_2~(2+)离子(硬酸)配位,溶液中形成3:1的配合物。Ⅰ_b与Hg~(2+)、Au~(3+)离子(软酸)配位形成2:1的配合物,用CNDO/2方法计算了各配体分子中原子净电荷密度和HOMO、LUMO能量。 相似文献
156.
Emulsion polymerization of methyl methacrylate (MMA) under pulsed microwave irradiation (PMI) with higher peak pulse power was studied. The effects of various parameters of PMI on the polymerization were analyzed and compared with that under conventional heating (CH) process. The results were summarized, as compared with that under CH, as follows. The amount of initiator used to reach constant conversion reduced by 50% at the same polymerization time; at the same initiator concentration 0.15 and 0.2 wt.%, the polymerization rate increased by 131% and 163%, respectively. The molecular weight of polymer obtained was 1.1-2.0 times larger than that under CH; at the same irradiation energy, the conversion achieved using a lower pulse power was greater than that using a higher pulse power. There seemed to be a factor of the irradiation energy efficiency; in other words, for the monomer conversion, the irradiation energy of low pulse power had a higher efficiency. The conversion achieved using a 3.5 μs pulse width was almost the same as that using a 1.5 μs pulse width. The results indicated that PMI had a significant non-thermal effect on the emulsion polymerization of MMA so as to effectively enhance the polymerization rate. The glass transition temperature (Tg), the polydispersity index (PDI) and the regularity of the polymer obtained using two processes were similar, indicating that the physical properties and microstructure of the polymer were not modified by the use of microwaves. 相似文献
157.
Feth MP Bolm C Hildebrand JP Köhler M Beckmann O Bauer M Ramamonjisoa R Bertagnolli H 《Chemistry (Weinheim an der Bergstrasse, Germany)》2003,9(6):1348-1359
XANES and EXAFS spectroscopic studies at the Mn-K- and Br-K-edge of reaction products of (S,S)-(+)-N,N'-bis(3,5-di-tert-butylsalicylidene)-1,2-cyclohexanediaminomanganese(III) chloride ([(salen)Mn(III)Cl], 1) and (S,S)-(+)-N,N'-bis(3,5-di-tert-butylsalicylidene)-1,2-cyclohexanediaminomanganese(III) bromide ([(salen)Mn(III)Br], 2) with 4-phenylpyridine N-oxide (4-PPNO) and 3-chloroperoxybenzoic acid (MCPBA) are reported. The reaction of the Mn(III) complexes with two equivalents of 4-PPNO leads to a hexacoordinated compound, in which the manganese atom is octahedrally coordinated by four oxygen/nitrogen atoms of the salen ligand at an average distance of approximately 1.90 A and two additional, axially bonded oxygen atoms of the 4-PPNO at 2.25 A. The oxidation state of this complex was determined as approximately +IV by a comparative study of Mn(III) and Mn(V) reference compounds. The green intermediate obtained in reactions of MCPBA and solutions of 1 or 2 in acetonitrile was investigated with XANES, EXAFS, UV/Vis, and Raman spectroscopy, and an increase of the coordination number of the manganese atoms from 4 to 5 and the complete abstraction of the halide was observed. A formal oxidation state of IV was deduced from the relative position of the pre-edge 1s-->3d feature of the X-ray absorption spectrum of the complex. The broad UV/Vis band of this complex in acetonitrile with lambda(max)=648 nm was consistent with a radical cation structure, in which a MCPBA molecule was bound to the Mn(IV) central atom. An oxomanganese(V) or a dimeric manganese(IV) species was not detected. 相似文献
158.
Spiro [3H-indole-3,2′-[4H] pyrido [3,2-e]-1,3-thiazine]-2,4′ (1H) diones, a class of previously unknown compound which does not form under conventional conditions, can be prepared by treatment of ‘in situ’ generated 3-indolylimine derivatives with 2-mercaptonicotinic acid under microwave irradiation in absence of any solvent or solid support in 85-92% yields in 3-8 min. The facile one pot reaction is generalized for a variety of ketones and amines to give pure pyrido [3,2-e] thiazine derivatives, which do not require further purification processes. 相似文献
159.
Marek Daszkiewicz Zbigniew Staszak Adam Pietraszko Wiesława Bronowska Maria Cieślak-Golonka 《Structural chemistry》2006,17(6):599-608
Two polymeric complexes: catena(μ-CrO4-O,O′)[Co(HIm)3H2O] (1) and catena(μ-CrO4-O,O′)[Co0.43Ni0.57(HIm)3H2O] (2) (where HIm=imidazole) with a cis-bridging coordination mode of the CrO4
2− anion have been synthesized and characterized by X-ray and spectroscopic methods. These crystals were isolated from nine
systems of varying reagent molar ratios and three excluding anions: Cl−, NO3
− and SO4
2− exclusively as mer [M(HIm)3O3]-type isomers. The unit cell of these isostructural complexes (monoclinic crystal system P21
/n) contains two independent helixes, left- and right handed, stabilized by intrahelical and interhelical hydrogen bonding and
π–π interaction between pairs of the imidazole rings from neighbouring helixes. The Raman spectra at 77 K of 1 and 2 deconvoluted into lorentzian components revealed the block-type polymeric structure of the complexes. Moreover, the solution
studies at millimolar concentrations of 1 and 2 indicated their complete decomposition in water. Four K electronic spectral analysis of the crystals (band deconvolution
into gaussian components) enhanced with the data obtained in the polarized light allowed for assignment of the bands to the
respective d–d transition (D4h symmetry). It was found that the metallic centres are independently absorbing species, which supports the suggestion of a
block-type structure of the polymers. The respective crystal field parameters for Co and Ni were calculated. 相似文献
160.
Novel visible-light-driven photocatalyst of NiO/Cd/g-C3N4 for enhanced degradation of methylene blue
《Arabian Journal of Chemistry》2020,13(6):5810-5820
Novel NiO/Cd/g-C3N4 photocatalysts were synthesized using a green and straightforward microwave-assisted method and characterized by X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), the Brunauer–Emmett–Teller (BET) method, transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), and ultraviolet–visible spectroscopy (UV–Vis). The ternary NiO/Cd/g-C3N4 nanocomposites were evaluated for the degradation of methylene blue (MB) at room temperature under the visible light irradiation. Experimental results revealed that the weight percent of cadmium had a remarkable effect on the photodegradation efficiency. The NiO/Cd/g-C3N4 (0.1%) sample exhibited superior activity in the degradation reaction. The activity of this nanocomposite was about 4.5 and 3.25 fold higher than those of the pure g-C3N4 and NiO/g-C3N4 samples in the degradation of MB, respectively. The enhanced photocatalytic activity was attributed to the low energy gap, increased absorption capacity of the visible light, and efficient suppression of the recombination of photogenerated electron-hole pairs. A detailed photocatalytic mechanism over the nanocomposite of NiO/Cd/g-C3N4 (0.1%) was proposed with superoxide radical anion O2– as the main reactive species. The stability of the nanocomposite was confirmed after four consecutive runs as well. 相似文献