5－（3，5－二溴－2－吡啶基）－1－（2－羟基－5－磺苯基）－3－（2－羟基苯基）甲的合成及其与铜显色反应的研究

介绍了显色剂５－（３，５－二溴－２－吡啶基）－１－（２－羟基－５－磺苯基）－３－（２－羟基苯基）甲（ＢＰＨＰＳ）的合成。详细研究了试剂与铜的显色反应，其灵敏度较高，摩尔吸光系数ε为２．４６×１０４。采用掩蔽方法，能显著提高体系的选择性。用拟定的方法测定了铜矿中的铜，结果令人满意。     

生物法苹果酸的合成与应用

介绍了生物法苹果酸Ｌ（－）－苹果酸的特殊性质，了共生产方法和分离方法，指出Ｌ（－）－苹果酸应用发展方向。     

24－表油菜素内酯中间体──（22E，24R）－3α－5－环－5α－麦角甾－22－烯－6－酮的合成

本文报道了以麦角甾醇（２）为起始物合成（２２Ｅ，２４Ｒ）－３α－５－环－５α－麦角－２２－烯－６－酮（１）的改进方法，化合物（１）是制备植物生长调节剂２４－表油菜素内酯（６）的关键中间体。     

全取代β—环糊精衍生物的合成

讨论了全烷基化β－环糊精的合成方法。用红外光谱研究了反应进行的程度。合成了七９２，３，６－三－Ｏ－甲基）－β－环糊精，七（２，３，６－三０－Ｏ－乙基）－β环糊精七（２，３，６－三－Ｏ－丙基）－β环糊精，七（２，３，６－三－Ｏ－丁基）－β－环糊精，七（２，３，６－三－Ｏ－戊基）－β－环糊精，七９２，３，６－三－Ｏ－辛基）－β－环糊精和七「３－Ｏ－甲基－２，６－二－Ｏ－（４－甲搓在甲基）」－β－环糊精     

2,5—二甲基—3,4—二乙酰基呋喃及其衍生物的合成

以ＫＩ－ＮａＩ为间接电解质，丙酮为溶剂，用间接电氧化的方法将乙酰丙酮（３）、乙酰乙酸乙酯（４）进行偶联反应，高产率地得到偶联产物四羰基化合物（５－６），进而在酸性介质中经Ｐａａｌ－Ｋｎｏｒｒ环化，合成了２，５－二甲基－３，４－二乙酰基呋喃（７）和２，５－二甲基－３，４－二乙氧羰基呋喃（８）。（７）再经ＮａＢＨ４还原得２，５－二甲基－３，４－二（１－羟基乙基）呋喃（９）。     

3—硝基—N—乙基咔唑单溴化反应的研究

研究了在不同的溶剂和后处理方式下３－硝基－Ｎ－乙基中文唑单溴化的三种方法：（１）冰醋酸－水稀释法；（２）冰醋酸－蒸馏法；（３）１，２－二氯乙烷－蒸馏法。比较了三种方法各自的优缺点，认为（３）法是较佳的工业化路线。     

高效液相色谱测定化妆品中的紫外线吸收剂

研究了用甲醇－甲氢呋喃－水作为流动相，从Ｃ１８柱上分离和测定羟苯甲酮－５－磺酸（ＭＳ４０）水杨酸钠，水杨酸苯酯（Ｓａｌｏｌ）羟苯甲酮（Ｍ４０）对－二甲酸氨基苯甲酸－２－乙基己酯（６００７）４－叔丁基－４－甲氧基二苯甲酸甲烷（１７８９）对－甲氧基肉桂酸－２－乙基己酯（ＭＣＸ），水氧酸－２乙基己酯（５８７）等８种紫外线吸收剂的色谱条件，建立了用ＨＰＬＣ测定上述物质的方法，其保留时间从２．８３ｍｉｎ（Ｍ     

手性双苯并咪唑化合物合成方法的改进

通过改进的Phillips方法用L（＋）－酒石酸、L（＋）－谷氨酸及L( )-天冬氨酸与邻苯二胺以盐酸盐形式在乙二醇中反应，合成了3种手性双苯并咪唑化合物（1R，2R）－二（2－苯并咪唑）乙二醇（HlbbImed);(1S),3-二（2－苯并咪唑）－1－丙胺（bbImpa),(1s),2-二（2－苯并咪唑）乙胺（bbImea)；反应产率比文献方法提高。还用KBH4分别测定了各手性化合物对苯乙酮和丁酮的不对称氢化反应性能。     

碳酸亚乙酯法生产乙二醇的展望

１非催化方法制乙二醇简介现阶段国内外乙二醇的工业生产方法大多是环氧乙烷（简称ＥＯ）直接水合法，这是一种非催化水合方法，主产品是乙二醇（简称ＥＧ），副产品是二甘醇（简称ＤＥＧ），三甘醇（简称ＴＥＧ）。主反应：ＥＯ＋Ｈ２Ｏ－－－－－－ＥＧ（１）副反应：Ｅ...     

原位荧光标定硝基化合物

介绍了用原位荧光标记法测定硝基化合物２，４－二氯苯基－４′－硝基苯基醚，Ｏ，Ｏ－二甲基－Ｏ－（３－甲基－４－硝基苯基）硫逐硫酸酯，Ｏ－乙基－Ｏ－异丙胺基－Ｏ－（对甲邻硝基苯基）硫逐磷酸酯，Ｏ，Ｏ－二甲基－Ｏ－（对硝基苯基）硫逐磷酸酯的方法，并报告了上述硝基化合物丹酰荧光衍生物的荧光性能。     

Cooperative enhancement of two-photon absorption based on electron coupling in triphenylamine-branching chromophore

Two novel, triphenylamine derivatives N-(4-(4-(diphenylamino)styryl)phenyl)acetamide and N-(4-(4-(bis-(4-(4-(diphenyl-amino)styryl)phenyl)amino)styryl)phenyl)acetamide were synthesized. The two-photon absorption of N-(4-(4-(bis-(4-(4-(diphenyl-amino)styryl)phenyl)amino)styryl)phenyl) was 17-fold greater relative to N-(4-(4-(diphenylamino)styryl)phenyl)acetamide. Linear absorption spectra, steady-fluorescence and time-resolved fluorescence spectra revealed that electron coupling originating from π-electron delocalization is responsible for the strong cooperative enhancement of TPA within the compounds. This is confirmed by the Lippert-Mataga equation.     

A novel organometallic ReI complex with favourable properties for bioimaging and applicability in solid-phase peptide synthesis

Organometallic complexes possess great potential for imaging applications in biology, due to their kinetic stability and often favourable intrinsic properties. In this work we present a new class of Re(I) -tricarbonyl complexes with a substituted bis(phenanthridinylmethyl)amine (bpm) ligand. The complex Re(CO)(3) (R-bpm) could be conveniently prepared by microwave synthesis from [Re(CO)(3)(H(2)O)(3) ]Br and a suitably substituted bis(phenanthridinylmethyl)amine (R-bpm). Complex 5, with R=CH(2)-CO(2)-CH(3) , was characterized by a single-crystal X-ray structure. Complex 6 (R=CH(2)-C(6)H(4)-CO(2)H) was used in solid-phase peptide synthesis (SPPS) to label the neurotensin(8-13) (NT) fragment N-terminally. The complexes show luminescence emission with large Stokes shifts (λ(ex) =350 nm, λ(em) =570 nm). Cellular uptake and intracellular localization studies in several cell lines demonstrate the utility of the new Re(CO)(3) (R-bpm) complexes for fluorescence imaging and reveal significant differences between the simple methyl ester 5 and the NT bioconjugate 7.     

11βHSD1抑制剂1-(4-三氟甲氧基苯甲酰基)-4-(4-甲氧基苯甲酰基)哌啶的合成研究

以4-甲氧羰基哌啶盐酸盐(1)和对三氟甲氧基苯甲酰氯(2)为起始原料,在三乙胺的作用下以92.7%的收率制得1-(4-三氟甲基苯甲酰基)-4-甲氧羰基哌啶(3);化合物(3)在羰基二咪唑与N,O-二甲基羟胺盐酸盐(4)作用下,以89.9%的收率制得1-(4-三氟甲氧基苯甲酰基)-4-(N-甲基-N-甲氧基羰基)哌啶(5);化合物(5)和4-甲氧基苯基溴化镁(6)偶联,以60.1%的收率制得化合物1-(4-三氟甲氧基苯甲酰基)-4-(4-甲氧基苯甲酰基)哌啶(7)。三步反应总收率50.0%。     

4,4′-联苯二乙酰丙酮桥联双核镍(Ⅱ)配合物的合成及磁性研究

以4,4′-联苯二乙酰丙酮和二苯甲酰甲烷为原料合成了标题化合物,并用元素分析、电导率、红外光谱、电子光谱和电喷雾质谱对其进行了表征,确定了配合物的组成,研究了配合物在氮气气氛中的热分解行为。其变温磁化率(2~300 K)的测定结果表明,桥联双核Ni2+配合物为铁磁性自旋交换作用,Curie常数C=2.04 cm3.mol-1.K,Weiss常数θ=8.10 K。     

Aspirin analogues as dual cyclooxygenase-2/5-lipoxygenase inhibitors: synthesis, nitric oxide release, molecular modeling, and biological evaluation as anti-inflammatory agents

Analogues of aspirin were synthesized through an efficient one-step reaction in which the carboxyl group was replaced by an ethyl ester, and/or the acetoxy group was replaced by an N-substituted sulfonamide (SO(2)NHOR(2):R(2) =H, Me, CH(2)Ph) pharmacophore. These analogues were designed for evaluation as dual cyclooxygenase-2 (COX-2) and 5-lipoxygenase (5-LOX) inhibitors. In vitro COX-1/COX-2 isozyme inhibition studies identified compounds 11 (CO(2) H, SO(2)NHOH), 12 (CO(2)H, SO(2)NHOCH(2)Ph), and 16 (CO(2)Et, SO(2)NHOH) as highly potent and selective COX-2 inhibitors (IC(50) range: 0.07-0.7 μM), which exhibited appreciable in vivo anti-inflammatory activity (ED(50) range: 23.1-31.4 mg kg(-1)). Moreover, compounds 11 (IC(50) =0.2 μM) and 16 (IC(50) =0.3 μM), with a sulfohydroxamic acid (SO(2)NHOH) moiety showed potent 5-LOX inhibitory activity. Furthermore, the SO(2)NHOH moiety present in compounds 11 and 16 was found to be a good nitric oxide (NO) donor upon incubation in phosphate buffer at pH 7.4. Molecular docking studies in the active binding site of COX-2 and 5-LOX provided complementary theoretical support for the experimental biological structure-activity data acquired.     

废铅酸蓄电池渣泥湿法脱硫和还原新工艺研究

对废铅酸蓄电池渣泥中硫酸铅脱硫和二氧化铅还原湿法过程进行研究。采用碳酸钠作脱硫剂，脱硫率比用碳酸铵要高。草酸作还原剂，还原率比亚硫酸盐等法要高。通过正交试验法，确定了硫酸铅脱硫过程的最佳工艺条件。通过单因素试验法，找出了二氧化铅还原过程的最佳工艺条件。     

Synthesis and biological activity of metabolically stabilized cyclopentyl trisphosphate analogues of D-myo-Ins(1,4,5)P3

We describe the synthesis of four novel metabolically stabilized analogues of Ins(1,4,5)P(3) based on the known cyclopentane pentaol tris(phosphate) 2: tris(phosphorothioate) 3, tris(methylenephosphate) 4, tris(sulfonamide) 5, and tris(sulfate) 6. Of these analogues, only the tris(phosphorothioate) 3 and parent tris(phosphate) 2 bound to the type I InsP(3)R construct. In addition, both the tris(phosphorothioate) 3 and parent tris(phosphate) 2 elicited calcium release in MDA MB-435 breast cancer cells. The Ins(1,4,5)P(3) agonist activities of these two compounds can be rationalized on the basis of computational docking of the ligands to the binding domain of the type I InsP(3)R.     

Synthesis and Aggregation of Novel Sugar-Based Gemini Surfactant with a N,N′-Acetylethylenediamine Spacer in Aqueous Solution

A novel sugar-based Gemini surfactant with a N,N′-acetylethylenediamine spacer (N,N′ (N-dodecyl-2-D-glucosaminyl acetyl) ethylenediamine, Glu(12)-(AA)-Glu(12)), was synthesized with D-(+)-Glucono-1,5-lactone as starting material in three steps. The surfactant's structure was confirmed using ¹H and ¹³C nuclear magnetic resonance (NMR) spectroscopy and electrospray ionization mass spectrometry (ESI-MS). The aggregation behavior of Glu(12)-(AA)-Glu(12) in aqueous solution at pH 4.0, 7.0, and 10.0 was investigated by surface tension, dynamic light scattering (DLS), and cryogenic transmission electron microscopic (Cryo-TEM) measurements. The surface tension measurement shows that the critical micelle concentration (CMC) of Glu(12)-(AA)-Glu(12) is at the concentration level of 10⁻⁵ mol·L⁻¹ at 25 °C, which is significantly lower than that of corresponding monomeric sugar-based surfactants. Compared with such sugar-based Gemini surfactants with similar hydrophilic spacers, Glu(12)-(AA)-Glu(12) demonstrated similar or slightly lower surface activity. The CMC value of Glu(12)-(AA)-Glu(12) underwent a slight decrease with the increase of pH. DLS and Cryo-TEM measurements reveal that Glu(12)-(AA)-Glu(12) forms micelles at acidic pH (pH 4.0) and the micelles are transformed into vesicles at neutral or high pH (pH 7.0, 10.0). The microstructural transformation of Glu(12)-(AA)-Glu(12) aggregates is related to the protonation state of its two tertiary amines in the head groups versus pH.     

Synthesis and Characterization of Some Novel Poly(nitroarylates)

Various types of poly(nitroarylates) ( 8 – 17 ) were prepared using interfacial polycondensation (IPC) and solution polycondensation (SPC) of 5-nitroiso-phthaloyl chloride ( la ) and 2-nitroterephthaloyl chloride ( 2a ) with different bisphenols: hydroquinone ( 3 ), resorcinol ( 4 ), 4.4′-dihydroxydiphenyl ( 5 ), 2,2-bis(4-hydroxyphenyl) propane ( 6 ) and bis(4-hydroxyphenyl) sulfone ( 7 ). A nitro group was introduced in the polymeric chain in order to improve the properties, solubility and thermal stability of these polymers. Some of the factors affecting the IPC were studied, such as the effect of concentration of the initial components and the role of the solvent. The structures of the poly(nitroarylates) ( 8 – 17 ) were confirmed by elemental analysis, infrared and proton magnetic resonance spectrometry. Thermomechanical analysis (TMA) and thermogravimetric analysis (TGA) of the synthesized polymers were also studied.     

Effect of Tb(III) on the properties of P(NIPAM-co-St) copolymer microspheres

Based on the synthesis of copolymer microspheres of N-isopropylacrylamide (NIPAM) and styrene (st) (P(NIPAM-co-St)), the interaction of Tb(III) and P(NIPAM-co-St) was investigated. It was found that when Tb(III) interacts with P(NIPAM-co-St) Tb(III) mainly bonds to O of the carbonyl group of P(NIPAM-co-St), forming the novel P(NIPAM-co-St)-Tb(III) complex. LCST, the zeta potential and the emission fluorescence intensity of P(NIPAM-co-St)-Tb(III) complex are different from P(NIPAM-co-St). Especially, after forming the complex, the intensities of the emission fluorescence peaks of Tb(III) at 487, 544 and 585 nm are enhanced 34, 35 and 17 times, respectively, comparing with that of the corresponding peaks of TbCl₃. Therefore, the P(NIPAM-co-St)-Tb(III) complex could transform the harmful ultraviolet radiation to harmless visible light. It is hoped that the results will provide a reference point for new applications of complexes of polymers and rare-earth elements, such as the P(NIPAM-co-St)-Tb(III) complex, in biomedicine and fluorescence systems.