Expeditious method for the synthesis of novel 2,3,5,6-tetrahydrobenzo[g][1,3,5]oxadiazocine-4-thiones linked with isoxazole

Synthesis of novel 3-aryl-5-（3,5-dimethylisoxazol-4-yl）-2,3,5,6-tetrahydrobenzo[g][1,3,5],oxadiazocine-4-thiones 5 has been accomplished from 3,5-dimethylisoxazol-4-amine 1 by condensation with salicylaldehydes, followed by reduction, treatment with aryl isothiocyanates and subsequent smooth ring closure via acetal formation in the presence of formaldehyde.     

Synthesis, crystal structure and luminescence properties of europium complexes with a new terpyridine-like ligand

New 1:1, 1:2 and 1:3 europium (Ⅲ) complexes with 2,4,6-tris(3,5-dimethylpyrazol-1-yl)-1, 3,5-triazine have been prepared, and their luminescence has been demonstrated to be sensitive to the π-π stacking and H-bonding interactions.     

Zinc-coordination Polymers Based on a Donor-acceptor Mix-ligand System: Syntheses,Crystal Structures and Photophysical Properties

By employing an electron-rich tricarboxytriphenyl amine as donor ligand and electron-deficient 2,4,6-tris(pyridin-4-yl)-1,3,5-triazine as acceptor ligand to assemble with Zn2+ions,three new coordination polymers were successfully synthesized and characterized systematically.Three compounds with different structures were obtained by regulating the reaction solvent,and the effect of the reaction solvent on the synthesis of crystals was explored.Furthermore,the photophysical properties of the compounds were investigated.     

Synthesis and crystal structure of nickel(Ⅱ) and zinc(Ⅱ) complexes with 2,4-bis(3,5-dimethylpyrazol-1-yl)-6-methoxyl-1,3,5-triazine

2,4-Bis(3,5-dimethylpyrazol-1-yl)-6-methoxyl-1,3,5-triazine(bpt) has been synthesized by using a new, simple and general method with high yields. Reactions of bpt with Ni(CIO4)2 · 6H2O and Zn(CIO4)2 · 6H2O in methanol gave mononuclear complex [Ni(bpt)2] · (CIO4)2 · H2O and ternary complex [Zn(mpt)2(dmp)](CIO4)2 respectively, where mpt (2,4-dimethoxy-6-(3,5-dimethyl-pyrazol-1-yl)-1,3,5-triazine) and dmp(3,5-dimethylpyrazole) are the alcoholysis products of bpt in the presence of Zn2+ ion. A possible mechanism for this catalytic reaction was proposed. X-ray crystal structure for ligand bpt, Ni and Zn complexes are reported. The protonated form of the ligand bpt crystallizes as its perchlorate salt including one molecule of water, [Hbpt · H2O · CIO4]. The proton is located on one pyrazole N-atom. [Hbpt ?H2O ?CIO4], in which [Hbpt]+ is in cis-cis conformation, are packed in slipped stacks of approximately parallel layers. The π-π overlap interactions between the non-protonized pyrazoles of the adjace     

Synthesis of a water-soluble macromolecular light stabilizer containing hindered amine structures

A novel water-soluble macromolecular light stabilizer was synthesized by grafting 2-chloro-4,6-bis- [(2,2,6,6-tetramethylpiperidin-4-yl)amino]-l,3,5-triazine onto polyvinylamine.The intermediate 2- chloro-4,6-bis-[(2,2,6,6-tetramethylpiperidin-4-yl)arnino]-1,3,5-triazine and the obtained macromolecular light stabilizer were characterized by ~1H NMR,HRMS,IR and UV spectroscopy.Cotton fabrics dyed with C.l.Reactive Yellow 145,C.I.Reactive Red 195 and C.I.Reactive Blue 19 were finished with the macromolecular light stabilizer,and the lightfastness of the dyes was tested.The results showed that the lightfastness of the reactive dyes was improved by 0.5-1.0 grade after being finished and the macromolecular light stabilizer exhibited good wash fastness and thermal stability.     

One Pot,Multi-component Synthesis of 3-[（4-Aryl-thiazol-2-yl）-hydrazono]-1,3-dihydro-indole-2-one

A series of 3-[（4-phenyl-thiazol-2-yl）-hydrazono]-1,3-dihydro-indole-2-one（4a-4g） and 3-{[4-（2-oxo2H-chromen-3-yl）-thiazol-2-yl]-hydrazono}-1,3-dihydro-indol-2-one（6a-6d） has been prepared in a one-step procedure from condensation reaction of isatin（1）,thiosemicarbazide（2） and bromoacetophenones（3）/or 3-（2-bromoacetyl）coumarins（4）.The method provides a simple and efficient route to prepare the compounds in good yields and in a short experimental time as compared to its stepwise procedure.     

Pi Stacking Interactions in Two TPT Derivatives and Their Photoluminescence Characters

π-π Stacking in the 2,4,6-tris（4-pyridyl）-1,3,5-triazine aromatic nitrogen-containing ligand and its metal-ligand complex Zn（TPT）2（H2O）4（OH）2 1 has been investigated by single-crystal X-ray diffraction analyses. The stacking mode of the ligand changes from the offset conformation to a perfect face-to-face alignment with the coordination to the zinc centers. The structure features are correlated with their solid-state luminescence properties. With excitation at 360 nm, free TPT ligand gives a strong fluorescent emission at 455 nm and the ligand-centered emission of the metal-ligand complex occurs at the same wavelength with lower emission intensity. The distance between the aromatic rings responds to the difference of luminescence characters.     

Synthesis of Eu（Ⅲ） and Tb（Ⅲ） Complexes with Two New Amide Type Podands and Their Luminescence Properties

Two new amide type podands L1 and L2 (L1=1,1,1-tris{[2-benzylaminoformyl)phenoxyl] methyl} propane,L2=1,3,5-timethyl-2,4,6-tris{[2-benzylaminoformyl)phenoxyl]methyl} benzene)and their europium and terbium nitrates complexes were synthesized.The luminescence properties of these complexes were also studied.     

Nitrogen-rich 6-（3,5-Dimethylpyrazol-1-yl）-3-（2,4,6-trinitroanilino）-1,2,4,5-tetrazin： Synthesis, Crystal Structure and Thermal Property

6-（3,5-Dimethylpyrazol-1-yl）-3-（2,4,6-trinitroanilino）-1,2,4,5-tetrazin （1） has been synthesized and characterized by ^1H NMR, MS, elemental analysis, infrared spectra and thermal analyses. The crystal structure was determined by X-ray diffraction method. 1 is crystallized in P21/c space group of monoclinic crystal system, and exhibits good physical properties, such as high densities （〉 1.55 g·cm^-3） and good thermal stabilities （Td〉220 ℃）. The intrermolecular hydrogen bonds construct the P- and M-helices from organic molecules and may contribute to the high melting points.     

Design,synthesis and biological estimation of 1-（benzoxazole-2-yl）piperazine and 4-（benzoxazole-2-yl）piperidine derivatives as potential α1-AR antagonists

Two series of 1-（benzoxazole-2-yl）piperazine （Sa-i） and 4-（benzoxazole-2-yl）piperidine compounds （10a-i） were designed, synthesized and evaluated for their α1-AR antagonistic activities. Biological assay in vitro indicated that 10h showed slightly stronger α1-AR antagonistic activity to that of our lead compound 1.     

Dichroism of absorption and polarization of phosphorescence of molecules of the closed form of nitrobenzospirothiopyran

The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997.     

非那雄胺合成工艺改进

非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。     

Determination of heats of detonation and influence of components of composite explosives on heats of detonation of high explosives

The heats of detonation of 20 simple high explosives and explosive mixtures were determined by means of an adiabatic detonation calorimeter designed by the authors. The results indicated that the performance of the instrument was reliable and the experimental data were very accurate. For explosive mixtures, there was a linear accumulative relationship between the heats of detonation of the explosive mixture and its components. Accordingly, the heats of detonation of explosive mixtures could be calculated directly from the heats of detonation of simple explosives and the characteristic heats of other components. The experiments showed that the gold or brass shell of the cylindrical charge could be substituted by a thick-walled porcelain shell, which had the advantage of cheapness.

     

恶臭嗅辨实验室建设探讨

针对恶臭测试的环境影响问题,提出了解决的实例方案,并对方案的要点及优缺点进行讨论,此方案在实际操作中具有较好的效果。     

Synthesis of phenolic components of Grains of Paradise

Two vanilloids, (5E)-8-(4-hydroxy-3-methoxyphenyl)oct-5-en-4-one (1) and 4-[3-hydroxydecyl]-2-methoxyphenol (2), isolated from the dried seeds of Grains of Paradise (Aframomum melegueta), were synthesized; the latter compound was made as the S-enantiomer and the material derived from the seeds was found to be a 1:1.7 mixture of the R and S isomers. The synthetic route used should allow the preparation of analogs having extended alkyl chains and consequently different lipophilicity, and 3, a homolog of 2, was also prepared.     

解决能源问题的新途径--光解水制氢的研究

面对日益枯竭的能源危机,氢能是一种洁净、最有前景的替代能源。目前在各种制氢的方法中光催化分解水制氢的研究最多,光解水过程中催化剂最关键,本文对利用太阳能光解水的途径、提高光催化反应效率以及光催化剂的开发研究进行了综述。     

氯氧化镁生成热的研究

用氧化镁氯化镁水溶液制备了8水合氯氧化镁[nMg(OH)2·MgCl2·8H2O], 并测定了其在盐酸中的溶解热, 实验结果表明, 氯氧化镁溶解热与n值呈线性关系, 根据溶解热求出5Mg(OH)2·MgCl2·8H2O和3Mg(OH)2·MgCl2·8H2O的生成热分别为-7727.1和5888.1kJ·mol^1^-。     

Summary of development of the theory of stability of colloids and thin films

In this review, the research of the author in the field of colloidal systems is summarized. The factors influencing colloidal stability are systematized and analyzed. Examples are presented to illustrate the practical utilization of the theory of stability of colloids and thin films.This review was prepared on the basis of the works of the author, which were awarded the State Premium for 1991 in the field of science and technology, chemistry section.Institute of Physical Chemistry, Russian Academy of Sciences, 117915 Moscow. Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 8, pp. 1708–1717, August, 1992.     

黄酮化合物的合成研究进展

黄酮化合物是一类具有多种生物活性的天然产物,其经典的合成方法主要为查耳酮路线和β-丙二酮路线.近年来出现了许多新技术、新方法.本文介绍了2'-羟基查尔酮的氧化关环法、黄烷酮氧化法、改进的Baker-Venkataraman法及其他合成黄酮化合物的方法.     

NiY分子筛表面酸性影响其选择性吸附脱硫性能的机理研究

采用原位红外光谱技术,以噻吩、环己烯和苯为模型探针分子,分别考察单一烃分子在NiY分子筛上的吸附与反应行为以及噻吩与烯烃、芳烃间的竞争吸附和催化反应行为。单一探针分子吸附研究发现,NiY分子筛中与Ni物种相关的Lewis(L)酸位是噻吩的选择性吸附活性位;噻吩和环己烯在NiY分子筛中Brnsted(B)酸位上发生的质子化和低聚反应明显弱于HY分子筛。双探针分子竞争吸附研究发现,环己烯二聚体在NiY中强B酸位上的强化学吸附与噻吩存在显著的竞争吸附行为。另外,苯和噻吩在NiY上的竞争吸附现象在373K时明显减弱。由此,在选择性吸附脱硫过程中,减少吸附剂表面B酸中心可降低烯烃对噻吩的竞争吸附,另外适当提高吸附体系的温度可以有效避免芳烃对噻吩的竞争吸附。