小檗碱与稀土硝酸盐二元配合物的合成、表征及抑菌作用

合成具有抑菌活性的稀土配合物,筛选具有抑菌活性的中药成分做有机配体合成稀土配合物.在乙醇溶液中合成了八种小檗碱与稀土硝酸盐的二元配合物,采用元素分析、红外光谱、差热-热重和X射线衍射等方法进行表征,确定配合物的化学组成为RE(NO3)3(B)3(RE=La3+,Sm3+,Nd3+,Dy3+,Pr3+,Y3+,Ce3+,Gd3+;B=C20H18NO4).研究了稀土配合物的抑菌活性,结果表明稀土配合物的抑菌效果较单独的稀土硝酸盐和小檗碱好.     

对叔丁基杯芳烃与稀土配合物的合成表征及抑菌活性

合成了对叔丁基杯[6]芳烃(H6L)及对叔丁基杯[8]芳烃(H8L′)与稀土RE(La,Sm和Tb)的配合物,通过元素分析、红外光谱进行表征,研究了这些配合物对高山红景天立枯丝核菌(Rhizoctonia solai Kuhn)和尖孢镰刀菌(Fusarium oxyporumSchlecht)的抑菌活性.结果表明,其配合物组成分别为[RE(H4L)(DMF)4(OH)].H6L和[RE(H6L′)(NO3)(DMF)4].2DMF(RE=La,Sm,Tb;H4L为电离出两个H 的H6L;H6L′为电离出两个H 的H8L′).配合物对这两种真菌均有较好的抑菌效果,浓度高则抑菌能力强,杯[8]芳烃稀土配合物的抑菌能力较杯[6]芳烃稀土配合物强.     

稀土(La,Ce,Er)-L-亮氨酸-邻菲啰啉三元配合物的合成及其抑菌活性

在乙醇-水介质中,经60℃水浴加热合成了三种稀土固体配合物。对其进行络合滴定、摩尔电导、元素分析、紫外光谱、红外光谱、热重-差热分析等测试,推测其化学组成为[Re(L-leu)3Phen]Cl3.nH2O,并对配合物进行大肠杆菌、金黄色葡萄球菌和枯草芽孢杆菌抑菌性质的测试;结果表明:LaCl3,CeCl3,ErCl3和L-亮氨酸没有抑菌效果,邻菲啰啉与三元稀土配合物对这三种菌都具有抑菌效果,但是三元稀土配合物的抑菌效果明显强于邻菲啰啉,而且对大肠杆菌抑菌效果更好。     

氨基喹啉水杨醛Schiff碱配合物的合成、晶体结构及抑菌性能

经缩合反应制备了4-甲氧基水杨醛缩-6-氨基喹啉希夫碱配体(L),并采用溶剂热法使其与Co(Ⅱ)、Zn(Ⅱ)和Cu(Ⅱ)三种金属离子进行配位得到配合物[Co L2](1),[ZnL_2](2)及[Cu L2](3),所得化合物结构通过元素分析、红外光谱、核磁共振谱及X射线单晶衍射法进行表征。生物测试结果表明,配体(L)及配合物1~3对马铃薯干腐病菌、苹果炭疽病菌、苹果腐烂病菌、番茄灰霉病菌4种植物病原菌具有较好的抑菌活性。     

微量热法测定粉防己碱金属配合物的抑菌性

从中药粉防己中提取粉防己碱。 在无水乙醇中粉防己碱分别与M(NO3)2·3H2O(M=Cu,Zn,Co,Ni)反应,合成了4种新的金属配合物,其结构分别用FT-IR和UV等测试技术进行了表征。 应用微量量热仪分别测定了不同浓度的粉防己碱及4种粉防己碱的金属配合物、M(NO3)2·3H2O(M=Cu,Zn,Co,Ni)对大肠杆菌代谢作用的热功率-时间曲线,运用Logistic方程计算出细菌的生长速率常数,建立了生长速率常数与药物浓度间的关系,进而确定了最佳抑菌浓度。 结果表明,4种金属配合物的抑菌作用均比M(NO3)2·3H2O和粉防己碱强。     

稀土硝酸盐与小檗碱固体配合物的合成,表征及抑菌效应研究

稀土硝酸盐与小檗碱固体配合物的合成、表征及抑菌效应研究刘宗怀张孟民张积强（宝鸡文理学院化学化工系７２１００７）小檗碱是由三颗针类植物中提取出来的季铵类生物碱，由于其具有较好的杀菌、消炎作用，已广泛应用于医学临床［１］，稀土硝酸盐也具有较好的消炎、杀菌...     

邻香兰素缩对甲苯胺Schiff碱稀土配合物的合成、晶体结构和热分解动力学机制

合成了2-甲氧基-6-[(4-甲基苯基)亚胺甲基]-苯酚Schiff碱(C15H15NO2,简写为HL)的3个稀土配合物[Pr(NO3)3(HL)2](1),[Nd(NO3)3(HL)2](2),[Er(NO3)3(HL)2]·0.5H2O(3),结构通过单晶X射线衍射分析确定,并用元素分析、摩尔电导、IR、1HNMR和紫外可见光谱进行表征。化合物1~3中,Schiff碱作为二齿配体与中心离子发生配位,稀土离子均采用十配位的双帽四方反棱柱构型,分别与两个Schiff碱中的4个氧原子、3个硝酸根中的6个氧原子发生配位。通过TG-DTG研究了配合物的热分解过程,用非等温动力学方法研究了配合物3的热分解动力学机制。     

膦酰基离子液体铕配合物的合成、结构与荧光性质

合成了两种膦酰基离子液体,1-丁基-3-(3-二苯基膦酰基)丙基咪唑六氟磷酸盐（[BIMC3P(O)Ph2]PF6）(IL-1)和(3-二苯基膦酰基)-丙基三乙胺六氟磷酸盐（[TEAC3P(O)Ph2]PF6）(IL-2),通过核磁共振和红外光谱确认了它们的结构,并合成了两种离子液体的稀土铕配合物Eu(IL-1)3(NO3)3和Eu(IL-2)3(NO3)3,对其进行了热稳定性和光谱性质的表征。 热重分析表明,离子液体的热稳定性均高于其稀土配合物,相比之下,离子液体IL-1和Eu(IL-1)3(NO3)3具有更好的热稳定性。 从红外光谱中可以看出,形成配合物后,两种离子液体中的P=O吸收峰均向低波数方向移动,同时两种配合物的紫外吸收强度均大于各自游离的离子液体,说明Eu3+和离子液体中的磷酰基发生了配位。 稀土铕配合物Eu(IL-1)3(NO3)3和Eu(IL-2)3(NO3)3的荧光光谱均表现出Eu3+的特征红光,峰形尖锐,单色性好,可作为潜在的红色发光材料。     

稀土对牙孢菌的抑菌机理研究

某些稀土盐类及其配合物抑菌性强、抑菌谱广,尤其对生命力极强的芽孢菌有 着更为突出的抑菌效果。本文的研究目的是探索稀土盐类及其配合物对芽孢菌的抑 菌机理;采用生物和化学方法,对芽孢进行破碎及成分的分离,借助电镜细胞化学 技术、红外光谱法、荧光分析法、原子吸收光谱法等检测手段,从分子水平上确定 了稀土离子在芽孢中的结合位点,提出了稀土对芽孢菌的抑菌机理是稀土离子取代 了芽孢内2,6-吡啶二羧酸钙(DPA-Ca~(2+))中Ca~(2+)的结合位点,形成了2,6-吡啶 二羧酸与稀土离子的配合物。     

稀土对牙孢菌的抑菌机理研究

某些稀土盐类及其配合物抑菌性强、抑菌谱广，尤其对生命力极强的芽孢菌有 着更为突出的抑菌效果。本文的研究目的是探索稀土盐类及其配合物对芽孢菌的抑 菌机理；采用生物和化学方法，对芽孢进行破碎及成分的分离，借助电镜细胞化学 技术、红外光谱法、荧光分析法、原子吸收光谱法等检测手段，从分子水平上确定 了稀土离子在芽孢中的结合位点，提出了稀土对芽孢菌的抑菌机理是稀土离子取代 了芽孢内2,6-吡啶二羧酸钙(DPA-Ca~(2+))中Ca~(2+)的结合位点，形成了2,6-吡啶 二羧酸与稀土离子的配合物。     

利用手持技术改进测定乙醇分子结构实验

利用压强传感器代替排水集气法,改进测定乙醇分子结构实验的仪器装置,并探索最佳反应条件。另外,设计两个空白实验,结合压强变化曲线对实验误差进行相关讨论。     

光谱仪测试范围的扩展

由于石化行业的生产需要，其材质的使用具有多样性和广泛性，经常会出现顾客委托的测试样品的一个或几个元素跨越光谱仪现有测试程序测量范围的情况。本法通过对光谱仪测试原理的认识，根据光谱仪的测试能力及标样的采集，实现了一个或几个元素测量范围的扩展，并对其测量的影响因素进行了研究。     

Neutral diterpenoids of oleoresins of five species of conifers of Transcarpathia

The compositions of the neutral diterpenoids of the oleoresins of five species of conifers growing in the Transcarpathia have been studied. It has been found that the oleoresins ofAbies alba M.,Larix decidua M., andPicea excelsa L. contain more than 50% of neutral diterpenoids. The group and qualitative compositions of the oxygen-containing diterpenoids have been determined. In the oleoresins ofAbies alba,Picea excelsa, andPicea abies tertiary alcohols — cis-abienol and isocembrol — predominate, while inLarix decidua the main component is the hydroxy ester larixyl acetate. Primary alcohols related to the resin acids have been found in all the oleoresins investigated. Features of the distribution of diterpenoids according to the species of conifers have been revealed. The results obtained are necessary for the chemotaxonomy of conifers of the family Pinceae.Novosibirsk Institute of Organic Chemistry, Siberian Branch, Academy of Sciences of the USSR. Translated from Khimiya Prirodynkh Soedinenii, No. 6, pp. 812–816, November–December, 1988.     

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.     

Influence of viscosity of medium on processes of oxygen quenching of excited states of mesoporphyrin

The oxygen quenching rate constants for singlet and triplet excited states of the dimethyl ester of mesoporphyrin IX increase with decreasing viscosity of the medium and reach a maximum at a viscosity of approximately 0.4 mPa·sec, after which the rate constants begin to decrease. The drop in rate constant with increasing fluidity of the medium may be related to a nonequilibrium character of the elementary act in the interaction of the reactants in the solvent cage. In viscous media such as isopropyl alcohol, isobutyl alcohol, and isoamyl alcohol, the reaction radius is greater than the sum of the radii of the reacting particles. The long-range character of these processes is due to the relatively weak dependence of the quenching probability on distance.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 25, No. 2, pp. 161–167, March–April, 1989.     

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.

     

物质分配系数的测定实验改进

实验教学目的是从解决实际问题出发,以实验技术训练和实验设计思想培养为目标。介绍了将单一的物质分配系数测定实验改进为综合实验,提高了实验效果及实验资源利用率。     

Calculation of enthalpies of hydrogenation of hydrocarbons

Sets of hydrogen molecule equivalents have been developed which permit the calculation of hydrogenation of different types of carbon-carbon bonds from ab initio total energies (3-21G and 6-31G* basis sets, and, to a more limited extent, for MP2/6-31G* data) of reactants and products. The calculated enthalpies of hydrogenation are in good agreement with experiment for unstrained molecules, with average errors on the order of 2 kcal/mol. The 6-31G* equivalents allow the enthalpies for strained molecules to be calculated accurately, but the 3-21G equivalents do not. The equivalents for both basis sets have been tested by calculating the enthalpies of hydrogenation of carbon-carbon bonds in nitrogen- and oxygen-containing organic molecules, free radicals, and classical carbocations. The results are in good agreement with experiment in most cases.     

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。