POLYMERIZATION OF N,N′-（PYROMELLITOYL）-BIS-L-LEUCINE DIACID CHLORIDE WITH HYDANTOIN DERIVATIVES BY MICROWAVE IRRADIATION

Facile and rapid polycondensation reactions of N,N′-(pyromellitoyl)-bis-L-leucine diacid chloride 1 with eight different derivatives of hydantoin compounds 2a-h were developed by using a domestic microwave oven in the presence of a small amount of polar organic medium such as o-cresol. The polycondensation reactions proceeded rapidly, compared with the conventional solution polycondensation, and was completed within 7-10 min, producing a series of novel optically active poly(amide-imide)s 3a-h with high yield and inherent viscosity of 0.35-0.65 dL/g. All of the above polymers were fully characterized by FT-IR, elemental analyses, inherent viscosity (ηinh), solubility test and specific rotation. Some structural characterization and physical properties of these optically active poly(amide-imide)s are reported.     

N—烯丙基—N′（对苯磺酸钠）硫脲与钯（Ⅱ）的显色反应及其应用

1 引 言N－烯丙基－N′－(对苯磺酸钠)硫脲(以下简写为NaNTU)是我们合成的一种新的硫脲类衍生物,性质稳定,易溶于水,无毒,具有很好的分析特性。从我们研究的36种离子与NaNTU的反应情况看,在1.7～4.2 mol/L的HNO3溶液中,只有钯*"能与NaNTU生成黄色络合物。据此,我们成功地将其用于钯*"的鉴定,取得了很好的效果。在此基础上,将该试剂首次应用于钯*"的光度分析,从而建立了光度法测定微量钯*"的新方法。研究表明,在1.7～４．2mol/L的HNO3溶液中,Pd2+和NaNTU形成一种稳定的摩尔比为1∶2的黄色水溶性络合物。络合物的最大…     

3-（4′-氯基苯基）-5-（2′-羧基偶氮）若丹宁催化动力学荧光光度法测定痕量锰

研究发现在pH5．2的邻苯二甲酸氢钾-氢氧化钠缓冲溶液中,Mn（Ⅱ）对过氧化氢氧化3-（4′-氯基苯基）-5-（2′-羧基偶氮）若丹宁的反应具有强烈的催化作用,并导致荧光强度的增加。据此建立了催化动力学荧光光度法测定痕量锰的方法,荧光强度的增加（△F）与Mn（Ⅱ）的质量浓度在o．014mg·L^-1以内呈线性关系,其线性回归方程为△F=-4．47＋1038．75C,相关系数为0．9886,检出限为1．78×10^-6g·L^-1。用于自来水和污水样品中痕量锰的测定,测得结果与原子吸收光谱法（AAS）的结果相符。分析结果的相对标准偏差（n=6）均小于2．5％,用标准加入法测得的回收率在95．6％～103．4％之间。     

N—取代苯基N′—（6—苯并噻唑基）脲类化合物的合成

为了寻找具有植物细胞激动素活性的新化合物,以苯并噻唑和取代苯胺为原料,将取代苯脲基引入到苯并噻唑的６－位上,合成了７个Ｎ－取代苯基Ｎ′－（６－苯并噻唑基）脲类化合物,它们的结构经元素分析、ＩＲ和＾１ＨＮＭＲ确定,７个化合物的合成收率分别为７４％,７６％,８５％,８２％,７０％,７３％和７２％。     

新显色剂N—烯丙基—N′—（氨基对苯磺酸钠）硫脲与金（Ⅲ）的显色反应

介绍了一种用新合成的显色剂Ｎ－烯丙基－Ｎ′－（氨基对苯磺酸钠）硫脲（ＡＳＡＴ）光度法测定微量金（Ⅲ）的方法。在ｐＨ３５～５５的ＨＡｃ－ＮａＡｃ缓冲体系中，该试剂和金（Ⅲ）形成一种稳定的水溶性配合物，其组成为ｎ（Ａｕ３＋）∶ｎ（ＡＳＡＴ）＝１∶２，配合物的最大吸收峰位于２９８６ｎｍ处，表观摩尔吸光系数为１１４×１０５Ｌ·ｍｏｌ－１·ｃｍ－１。Ａｕ３＋量在７２～５６８μｇ／Ｌ服从比尔定律，相关系数ｒ＝０９９９３。将该法应用于金矿石中微量金的测定，获得满意的结果。     

用N—苯基—N′—（氨基对苯磺酸钠）硫脲光度法测定微量钯（Ⅱ）

１引言 硫脲类化合物作为显色剂测钯已有报道,氨基硫脲及其衍生物分子中,含有的氮、硫两种原子均可作为电子的给予体,提供电子对与多种金属离子生成金属资合物,因而广泛应用于金属离子的定性、定量分析。本实验室合成的系列氨基硫脲类化合物已成功应用于钯的定量分析。本文研究了新的水溶性试剂Ｎ－苯基－Ｎ’－（氨基对苯磷酸钠）硫脲（ＰＰＴ）与钯（Ⅱ）的显色反应,通过寻找适宜的反应条件,建立了测定微量把（Ⅱ）的新方法。该法灵敏度高、操作简便,且测定结果准确可靠。将该法用于废催化剂中把的测定,所得结果令人满意。２实验…     

Synthesis and Crystal Structure of Bis（nitrate）bis（N—n—octyl—α—pyrrolidone）uranyl（Ⅱ）

The crystal structure of the title compound UO2(NO3)2[CH2(CH2)2CONC8H17] was determined by single-crystal X-ray diffraction. Crystal data: triclinic, space group P ī, a = 7.456(2), b = 8.371(2), c = 13.470(3)A, α = 95.66(1), β = 94.64(2), γ = 102.67(2)°, C24H46N4O10U, Mr = 788.68, V = 811.73A3, Dc = 1.613 g/cm3, Z = 1, F(000) = 390, μ = 5.052 mm-1, the final R = 0.0256 and wR = 0.0568 for 2826 observed reflections I>2σ(I). The central uranyl ions are coordinated by six oxygen atoms. Two of them are from the carbonyl groups of N-octyl--pyrrolidone molecules, and the other four from two nitrate groups.     

Synthesis and Structure Characterization of Aqua-（μ2-carbonato-O,O′）-（2,2′-bipyridyl）-copper（Ⅱ） Dihydrate

Under hydrothermal conditions the reaction of cis-aconitic acid with Cu2(OH)2CO3 and bipy (bipy = 2,2'-bipy) in H2O/DMF (3:2) afforded a neutral mononuclear compound [Cu- (bipy)((2-CO3)(H2O)](2H2O, which has been structurally characterized by single-crystal X-ray diffraction analysis. The crystal belongs to triclinic, space group Pī with a = 8.3950(5), b = 8.7974(5), c = 9.4496(3)（A。）, α = 98.270(3), β = 93.014(3), γ = 100.068(3)°, V = 677.83(6) （A。）3, Dc = 1.635 g/cm3, Z = 2, C11H14CuN2O6, Mr = 333.78, μ = 1.637 mm－1, λ(MoKα) = 0.71073 （A。）, F(000) = 342, the final R = 0.0616 and wR = 0.1273 for 1621 observed reflections with I > 2σ(I). The structure of the complex contains a distorted square pyramidal core with a bipy, a carbonate anion and a water molecule coordinating to a CuⅡ atom. The dihedral angle between the two planes composed of N(1)N(2)Cu(1) and O(1)O(3)Cu(1) is 21.73(8)°. The intermolecular hydrogen bonds (O…O) are observed in the crystal structure.     

N，N′—1，2—丙水杨酰胺合铜（Ⅱ）酸根的双核Cu（Ⅱ）配合物的合成与磁性

合成了一类新的金属配合物[Cu(sampn)CuL](sampn^4-:N，N′－1，2－丙水杨酰胺根离子；L：2，2－联吡啶或1，10－菲绕啉），经元素分析、IR、电子光谱等手段推定配合物具有酚氧桥结构，Cu（Ⅱ）离子和配位环境为畸变四方构型，测定了配合物的变温磁化率，其数值用量二乘法与修正的Bleaney-Bowers方程拟合，从中得到较大的θ值，表明双核分子间有较大的分子间相互作用。     

Study on the Surface Photovoltage and Fluorescence Properties of N,N′—Bis（4′—aminopheny）—1,4 quinonenediimine Doped with H4SiW12O40

Aniline oligomer composite materials using heteropolyacid H4SiW12O40 as dopant was synthesized, and the effect of the doping concentration on the photoluminescence and surface photovoltain properties were investigated.     

Microwave promoted one-pot synthesis of 3-(2′-amino-3′-cyano-4′-arylpyrid-6′-yl)coumarins

A facile procedure for the synthesis of 3-(2′-amino-3′-cyano-4′-arylpyrid-6′-yl)coumarins are being reported starting from 3- acetylcoumarin,aromatic aldehydes and malononitrile.The reactions were carded out on microwave irradiation in good yield with short time and easy work-up.The structures of all the compounds have been confirmed on the basis of their analytical,IR,~1H NMR, and mass spectral data.