AMPA受体拮抗剂NS1209的合成

以5-溴异喹啉为起始原料,经过9步反应合成了AMPA受体拮抗剂——NS1209,总产率37.3％,其结构经1H NMR和MS确证.     

由5-羟基-1,3-苯二酸构筑的A2B型单体合成新的一类聚醚树状物

我们以5-羟基间苯二甲酸为起始原料，通过酯化、酚羟基保护、还原、氧化、Wittig反应延长碳链、再还原、溴代等步骤合成了A₂B型长链单体，用它通过收敛法合成了表面基团为甲酯、内部为苄氧基的新型一至三级聚醚类树状化合物。对部分树状物的表面基团进行了转化，使其外围接上萘环，并对它们的紫外吸收和荧光光谱进行了研究。     

An Efficient Solid-State Synthesis of N-Aryl-2-phenyldiazenecarboxamides

The subject of organic solid-state synthesis is a fascinating one. It has many advantages such as high efficiency and selectivity, easy separation and purification, mild reaction conditions, and environmental acceptability1. In recent years, this method has been widely used in a variety of organic reactions including substitution2, condensation3, oxidation-reduction4, rearrangement5 and elimination6. However, the solid state reaction using K3Fe(CN)6/KOH to oxidize substituted semicarbazides…     

Synthesis of New Potential NMDA Antagonist Based on Acylphosphonate Derivatives

Abstract

In recent years intensive pharmacological research is focused on the N-methyl-D-aspartate (NMDA) receptor, which has been implicated in normal neuronal hnctioning, including excitatory synaptic transmission, as well as in the pathologies of the central nervous system such epilepsy, Alzheimer and Parkinson's disease, and neurodegeneration following a stroke.     

A Series of Analogues to the AT2R Prototype Antagonist C38 Allow Fine Tuning of the Previously Reported Antagonist Binding Mode

We here report on our continued studies of ligands binding to the promising drug target angiotensin II type 2 receptor (AT₂R). Two series of compounds were synthesized and investigated. The first series explored the effects of adding small substituents to the phenyl ring of the known selective nonpeptide AT₂R antagonist C38 , generating small but significant shifts in AT₂R affinity. One compound in the first series was equipotent to C38 and showed similar kinetic solubility, and stability in both human and mouse liver microsomes. The second series was comprised of new bicyclic derivatives, amongst which one ligand exhibited a five-fold improved affinity to AT₂R as compared to C38 . The majority of the compounds in the second series, including the most potent ligand, were inferior to C38 with regard to stability in both human and mouse microsomes. In contrast to our previously reported findings, ligands with shorter carbamate alkyl chains only demonstrated slightly improved stability in microsomes. Based on data presented herein, a more adequate, tentative model of the binding modes of ligand analogues to the prototype AT₂R antagonist C38 is proposed, as deduced from docking redefined by molecular dynamic simulations.     

Voltammetry as the First Method for Direct Determination of a Novel Antagonist of A2A Adenosine Receptors

In this article, for the first time, the analytical method for determination of a novel antagonist of A_2A adenosine receptors (8‐(4‐methoxyphenyl)‐4‐oxo‐4,6,7,8‐tetrahydroimidazo[2,1‐c][1,2,4]triazine‐3‐carbohydrazide, namely IMT), which can be used as a drug for liver diseases, was presented. For this purpose a commercially available boron‐doped diamond electrode (BDDE) in combination with differential pulse voltammetry (DPV) was applied. It was found by cyclic voltammetry (CV) that IMT displays at BDDE, as a sensor, two well‐defined oxidation peaks at potentials of 0.81 and 1.18 V and one reduction peak at 1.1 V vs. Ag/AgCl in 0.1 mol L^?1 acetate buffer (pH 4.5±0.1). The oxidation and reduction mechanism of IMT was proposed. The developed DPV method allowed the successful determination of IMT in the range of 0.05–50 μmol L^?1 with detection limit equal to 0.0094 μmol L^?1 and without any chemical modifications and electrochemical pretreatment of the electrode surface. The proposed procedure allows the determination of IMT in vitro directly from urine samples.     

Efficient Synthesis of Olmesartan Medoxomil,an Antihypertensive Drug

This document describes a simple and robust process for the synthesis of olmesartan medoxomil. This tailored process allows us to synthesize olmesartan medoxomil on a large scale with 50% overall yield. Also, our process has excellent control of the impurity profile in all the stages.     

不同形态SnO2纳米晶的制备

In this paper, we report our research on morphologically selective synthesis of nanocrystalline SnO2 by the combination of hydrothermal preparation and calcinated process. We firstly prepared SnO2 nanocrystals by the hydrothermal method at 140 ℃ for 3 h, using SnCI4 as the reactant. With the initial pH of 1.8 or 1.34, we prepared uniform and well-dispersed SnO2(tetragonal) nanocrystals, with similar size of about 3 nm, as determined by TEM. However, after being calcinated at 500 ℃ for 2 h, specimen 1 prepared at pH＝1.8 showed the rod-like shape with an average size of 5 nm×20 nm, while the other one(specimen 2)prepaed at pH＝1.34 showed a granular shape with an average size of 10 nm. XRD experiments showed that specimen 1 had a new diffraction peak after calcination, which was contributed by the (023) face of orthorhombic SnO2. The experiment results indicated that the morpholgy of SnO2 nanocrystals after calcination was closely related to the initial acidity of the reaction solution, possibly due to the difference in surface properties, e.g. the difference in crystalline faces exposed to the surface of particals, under different hydrothermal conditions.     

N-二异丙氧磷酰化氨基酸的合成

以亚磷酸二异丙酯为磷酰化试剂、次氯酸钠为氯代试剂首次对20种常见的α-氨基酸进行了磷酰化.通过添加适量四丁基溴化铵为相转移催化剂,使用过量的亚磷酸二异丙酯以补偿其在强碱环境中的水解,从而提高了反应产率.所得产物经核磁共振谱、红外光谱和质谱鉴定结构并分析总结了该类化合物的谱图特征规律.     

Highly Efficient One-Pot Synthesis of 2-Aminobenzoxazoles Using Triflic Acid as a Cyclodesulfurizing Reagent

An efficient one-pot synthetic strategy for 2-aminobenzoxazoles was developed from isothiocyanates and 2-aminophenol using triflic acid as a cyclodesulfurizing reagent.

三苄基锡(IV)炔基(烯基)膦酸衍生物的合成及结构表征

烃基锡的膦（磷）酸衍生物具有较强的杀虫、杀菌及除草等生物活性,受到人们的极大关注［１,２］,尤其是三烃基锡（ＩＶ）二硫代磷酸酯的合成及应用研究已有较多报道［３,４］,但三烃基锡（ＩＶ）膦酸衍生物的合成研究很少［５］,而三烃基锡（ＩＶ）不饱和烃基膦酸衍生物Ｒ３ＳｎＯＰ（Ｏ）（ＯＨ）Ｒ’（Ｒ’为炔基或烯基）的研究尚未见文献报道。我们以三苄基氯化锡和炔基（烯基）膦酸单钠为原料,合成了６种三苄基锡（ＩＶ）炔基（烯基）膦酸类化合物。并用元素分析、红外光谱、核磁共振、氢谱和锡谱、质谱及热重分析等手段表征了这些化合…     

Efficient Synthesis of 2-Arylamino-2-imidazolines and 2-Ami-nobenzimidazoles with Aminoiminomethanesulfonic Acid Derivatives

A highly efficient synthesis of 2‐arylamino‐2‐imidazolines and 2‐aminobenzimidazoles from aminoimino‐methanesulfonic acid derivatives is described. The method is simple and practical, generating imidazoline and benzimidazoline derivatives in excellent isolated yields.     

新型2-苯并噻唑磺酰脲氨基酸及其甲酯衍生物的合成与抗肿瘤活性

以2-巯基苯并噻唑为原料,经弱氧化和氨化制得2-苯并噻唑次磺酰胺（2）; 2经高锰酸钾氧化制得2-苯并噻唑磺酰胺（3）; 3与氯甲酸乙酯反应制得2-苯并噻唑磺酰胺甲酸乙酯（4）; 4与L-氨基酸甲酯反应制得一系列2-苯并噻唑磺酰脲氨基酸甲酯（6a~6j）; 6经水解合成了10个新型的2-苯并噻唑磺酰脲氨基酸（7a~7j）,其结构经¹H NMR, IR和ESI-MS表征。并研究了6和7对Cdc25B的抑制活性。结果表明:在用药浓度为20 μg·mL^-1时,6c, 6j, 7d, 7h和7j对Cdc25B抑制活性较好,抑制率分别为78.1%, 71.2%, 65.6%, 57.2%和65.9%。     

Synthesis of an o-Nitrobenzyl Attached A1 Adenosine Receptor Antagonist,a Prodrug Approach

Abstract

The o-nitrobenzyl group, possessing distinct advantage of being photolabile under mild conditions, was successfully connected to 8-(5,6-epoxynorbornan-2-yl)-1,3-dipropylxanthine (5), a high specific A₁ adenosine receptor antagonist. The resulting compound 4 would have potential use as a prodrug.     

新型苯并吡喃类FSH拮抗剂的合成

以2-溴-4,5-二甲氧基苄溴为起始原料,依次经取代、Sonogoshira偶联、水解、酰化和氧化反应合成了新型FSH拮抗剂——(R)-N-[1-羟基-3-(1H-吲哚-3-基)丙烷-2-基]-3-异丙氧基-8,9-二甲氧基-6H-苯并[c]苯并吡喃-2-甲酰胺,总收率16.8%,其结构经~1H NMR和MS(ESI)确证。     

三苄基锡(IV)炔基(烯基)膦酸衍生物的合成及结构表征

Six novel tribenzyltin(IV) dervatives of alkynyl or alkenyl Phosphonic acid (PhCH₂)₃SnOP(O)(OH)R, Where R=C≡CPh, C≡CC₃H₇ n,C≡CC₄H₉ n, C≡CC₅H₁₁ n,C≡CC₆H₁₃ n, CH=CClPh,were synthesized by resaction of the monosodium salt of the alkynyl or alkenyl phosphonic acid with tribenzyltin(IV) chloride in benzene. Their structures were cheracterized by elementary analysis, IR,¹H NMR, ¹¹⁹Sn NMR, MS and TG DTA. The results showed that these compounds arefive coordinated -O-P-O-bridged polymers.     

新的氨基酸受体的合成和分子识别性质研究

从双氨基甲基手性双环胍出发,经三步反应合成了由稳定的共价键桥联双环胍、氮杂冠醚和萘环的氨基酸受体1.液-液竞争萃取和^1HNMR实验表明受体对氨基酸两性离子具有较好的侧链选择性和对映选择性,能够选择性地将L-芳香族氨基酸从水相转移到二氯甲烷有机相。