对二氟甲氧基乙酰苯胺的制备新工艺

对二氟甲氧基乙酰苯胺(1)是一种重要的药物中间体,可用于多种医药、农药等的合成,如用于新型胃药及除虫菊类杀虫剂的合成,尤其进入80年代以来,许多专利报道其用于新药合成[1～6].     

微波辐射条件下对氯硝基苯和酚盐的反应

近年来 ,微波技术在化学领域中的应用不断扩大。国内外有不少综述和应用的报道 ,在许多有机反应 ,如缩合[1 ] 、取代[2 ] 、重排[3] 、氧化[4] 、还原[1 ] 中 ,都有应用微波技术的报道。在微波辐射条件下 ,许多反应缩短了反应时间 ,增加了反应的选择性 ,提高了反应的收率 ,甚至使原来一些难以进行的反应得以顺利进行[5] 。在合成化学上 ,微波技术已经展现出很好的应用前景。硝基二苯醚类化合物是一类很重要的化合物 ,被广泛应用于农药、染料、颜料、医药和橡胶助剂等领域[6] ,其经典的合成方法是Ｕｌｌｍａｎ法或Ｗｉｌｌｉａｍｓｏｎ法[7～…     

合成正丁基磺酰氯的新方法

合成正丁基磺酰氯的新方法党占青康汝洪（石家庄师专化学系０５００４１）（河北师范大学化学系石家庄０５００１６）烷基磺酰氯是酯化、聚合的催化剂，油墨、涂料的固化剂，染料、医药、农药等的重要化工原料。其合成方法已有许多报道，文献￣［１－１６］是以硫醇、二烷...     

高效液相色谱法测环糊精

环糊精在医药、食品、化学、轻工.金属和石油采矿等许多行业中有广泛的用途。国外曾用分光光度法、质谱法.X射线衍射法及高效液相色谱等方法测定环糊精。其中高效液相色谱法作为分离分析的手机.较其它几种方法更为简便。用高效液相色谱法测环糊精,国外已报道的有纤维素分配色谱法、活性炭吸附色谱法、交联葡萄糖凝胶、     

(S)-1-苯基-1,2-乙二醇的合成

手性醇作为重要中间体可广泛用于药物﹑农药及食品添加剂等的合成,国内外已有许多相关的合成报道[1,2].二元手性醇具有光、热和化学稳定性,是材料科学及药物开发的重要原料,如(S)-1-苯基-1,2-乙二醇,它不仅是液晶中不可缺少的重要原料和手性添加剂,而且已成为制备具有光学活性的医药、农药和功能材料的重要中间体[3,4].     

4-氟苯甲醛丙氨酸席夫碱的合成及其IR和Raman光谱分析

席夫碱及其金属配合物具有杀菌、抗菌、植物生长调节等生理活性,在医药、农药等领域有广泛的应用前景[1-2].含氟席夫碱及其配合物具有独特的生物活性, 在医药研究中备受关注[3-4]; 氨基酸席夫碱一直是人们感兴趣的研究课题,但对含氟的氨基酸席夫碱的研究未见报道.本文报道了4-氟苯甲醛与丙氨酸形成的席夫碱的合成方法及利用1H NMR、红外光谱、拉曼光谱、热重分析等测试手段进行表征的结果,化合物的生物活性研究正在进行.     

2-芳基-5-(2-苯基-4-喹啉基)-1,3,4-恶二唑衍生物的合成及其相关性质的研究

1,3,4-恶二唑衍生物在医药,农药、染料、涂料、高分子合成材料以及有机闪烁体材料等方面有广泛用途。近年来有关合成和生理活性的研究报道甚多。本文选择被淘汰的解热镇痛、去风湿药物     

静态法和动态法测量乙醇饱和蒸气压的比较

物质的蒸气压是化学、化工、冶金、医药等领域的重要基础数据。测量饱和蒸气压是大学物理化学实验教学中的一个基础实验,测量方法主要有静态法和动态法,但两种方法的比较尚未见报道。本文通过比较,得出了两种方法的优缺点以及注意事项。     

扁桃酸在玻碳电极上的电化学行为研究

扁桃酸(mandelicacid)具有较强的抑菌作用,可用于治疗泌尿系统疾病,同时也是合成许多抗生素药物的中间体.因此,它在医药合成中具有广泛的用途.对扁桃酸的测定,已有紫外、HPLC、气相色谱、毛细管电泳等方法报道;电化学法测定还未见报道.本文采用现代电化学分析方法系统研究了扁桃酸在玻碳电极上的电化学行为.实验表明扁桃酸在玻碳电极上的氧化是不可逆过程,在pH 2.0介质中,在玻碳电极上都有一定的吸附性.实验研究了在pH 2.0条件下扁桃酸的各种电化学性质,并分别寻找到在不同条件下的定量方法,对实际样品进行了测定,方法简便、快速.     

SiO_2包覆超细CaCO_3的微晶分析和XPS研究

0引 言 超细碳酸钙在橡胶、塑料、造纸、涂料、油墨、医药、化妆品等工业中有广泛应用。碳酸钙粉末表面具有许多水羟基,表面是亲水疏油性的 ,易形成聚集体 ,分散性能差 ,直接应用效果不好。因此,根据其本身的性质及其应用目的,对其进行表面处理,以相应提高其应用性能。碳酸钙的表面处理是通过物理或化学方法将表面处理剂吸附或反应在碳酸钙的表面,形成表面改性层,使其表面活性化,以改善碳酸钙的表面性能。目前碳酸钙的表面改性大多为有机表面改性、偶连剂表面改性、高分子（聚合物）表面改性等 [1],而无机表面改性却很少有报道。我…     

A simple and efficient method for synthesis of fluorine-containing saccharide esters and antiviral activity

Sixteen new fluorine-containing saccharide esters from fluorine-containing benzoic acids and α-O-acetylglycosyl bromide were synthesized in the presence of 4-dimethylaminopyridine (DMAP) and triethylamine (Et₃N) under mild conditions in good yields and their structures were clearly verified by IR, ¹H NMR, MS and elemental analysis. This method has high stereospecificity, the configuration is unitary, the new synthesized compounds are all of β-configuration. The results of bioassay showed that these title compounds possess potential antiviral activities against tobacco mosaic virus (TMV).     

新型一枝蒿酮酸异噁唑衍生物的合成及其抗A,B型流感病毒活性研究

为了提高一枝蒿酮酸的生物活性,以一枝蒿酮酸和3-取代苯基-5-氨甲基-异噁唑为原料,在偶合试剂DCC,HOBt/DMAP的作用下,合成了6个未见文献报道的含异噁唑的一枝蒿酮酸酰胺衍生物3a～3f.所合成的化合物均经过IR,1H NMR,13C NMR,ESI-MS等分析方法表征及初步体外抗A(H3N2,H1N1)型和B型流感病毒活性研究.初步实验结果表明:化合物3c同时具有抗A(H3N2)型和B型流感病毒活性,化合物3c和3e表现出比母体化合物强的抗B型流感病毒活性.     

Solid‐phase extraction of phenoxyacetic acid herbicides in complex samples with a zirconium(IV)‐based metal–organic framework

A zirconium(IV)‐based metal–organic framework material (MOF‐808) has been synthesized in a simple way and used for the extraction of phenoxyacetic acids in complex samples. The material has good thermal and chemical stability, large specific surface area (905.36 m²/g), and high pore size (22.18 Å). Besides, it contains a large amount of Zr‐O groups, easy‐to‐form Zr‐O‐H bond with carboxyl groups of phenoxyacetic acids, and possesses biphenyl skeleton structure, easy to interact with compounds through π‐π and hydrophobic interactions. These characteristics make the material very suitable for the extraction of certain compounds with a high extraction efficiency and excellent selectivity. The extraction conditions were optimized, and then an analytical method was successfully established and applied for analysis of actual samples. The solid‐phase extraction method based on prepared material had a wide linear range of 0.2–250 μg/L and a low detection limit of 0.1–0.5 μg/L for four phenoxyacetic acid compounds including 2,4‐dichlorophenoxyacetic acid, 2‐(2,4‐dichlorophenoxy) propionic acid, 4‐chlorophenoxyacetic acid, and dicamba. The relative standard deviations of intra‐ and interday precision were 1.8–3.8 and 4.3–6.9%, and the recoveries after spiking were between 77.1 and 109.3%. The results showed that the material is a desired substituent for the extraction of compounds with benzene ring structure containing carboxyl groups.     

脂氧合酶模型化合物[Fe(CTB)Cl]Cl·3CH3CH2OH·H2O的合成、晶体结构与氧化活性

合成了含Fe2+的脂氧合酶模型化合物[Fe(CTB)Cl]Cl.3CH3CH2OH.H2O(CTB为N,N,N,'N'-四(2'-苯并咪唑甲基)邻二胺反式-环己烷).该配合物属单斜晶系,P21/n空间群.晶胞参数a=1.12938(7)nm,b=1.49004(9)nm,c=2.69346(17)nm,β=91.9530(10),°V=4.5300(5)nm3,Z=4;R=0.0602,wR=0.1629.中心离子Fe2+只与六齿配体CTB的3个苯并咪唑的3-位氮和两个烷胺氮配位,氯离子占据着第六配位位点,整个配合物呈变形八面体构型.该化合物可催化亚油酸氧化断链成丙二醛(酸)、壬烯醛和壬醛酸等低分子醛和ω-氧酸.     

双环笼状磷酸酯的研究(Ⅱ)——1-硫代-1-磷杂-2,6,7-三氧杂双环[2,2,2]辛烷-4-甲撑衍生物的合成

本文合成了1-硫代-1-磷杂-2,6,7-三氧杂双环[2,2,2]辛烷-4-甲撑膦酸酯新化合物11个.发现只有在三乙胺和DMAP同时存在时,1-硫代-1-磷杂-4-羟甲基-2,6,7-三氧杂双环[2,2,2]辛烷方可顺利进行磷酰化得到产物.探讨了DMAP的强有效的催化作用机制.生物初筛表明部分化合物对植物生长有调节作用.     

2-取代-3-N-酰基-5-氟-4-嘧啶酮的合成及其抗肿瘤活性

在丙酮溶液中,于Et3N存在下使2-取代-5-氟-4-嘧啶酮与酰氯反应,合成了14个未见文献报道的2-取代-3-N-酰基-5-氟-4-嘧啶酮类化合物,它们的结构经IR,1H NMR,元素分析或MS确定.其中有些化合物具有一定的抗肿瘤活性.     

Synthesis of and tautomerism in 3-acyltetramic acids

The synthesis of 3-acyltetramic acids, the substructure of bioactive natural products, via O-acylation of tetramic acids with carboxylic acids followed by acyl migration, has been investigated. This acylation sequence is mediated by N,N'-dicyclohexylcarbodiimide (DCC) and 4-dimethylaminopyridine (DMAP) and is very sensitive to the nature of the nitrogen substituent (R(1)), the nature of the carboxylic acid (R(2)CO(2)H), and the amount of DMAP. Acylation of N-acyl tetramic acids with an alkyl carboxylic acid using 1.3 equiv of DMAP (with 1.1 equiv of DCC) unexpectedly gave the 3-acyltetramic acid directly as a result of acyl migration induced by excess amounts of DMAP. On the other hand, N-unsubstituted, N-alkyl, and N-acyl tetramic acids with alkyl and aromatic carboxylic acids gave the O-acyl tetramic acids by using only 0.1 equiv of DMAP (with 1.1 equiv of DCC); these could be further rearranged to the acyl product by treatment with excess DMAP. The tautomeric equilibrium of these 3-acyltetramic acids in solution was found to strongly depend on the nitrogen substituent group (R(1)) rather than the 3-acyl group.     

Preparation and pharmacological evaluation of novel glycoprotein (Gp) IIb/IIIa antagonists. 1. The selection of naphthalene derivatives

The synthesis and design using molecular modeling techniques for non-peptide, low molecular weight novel fibrinogen receptor (glycoprotein IIb/IIIa: Gp IIb/IIIa) antagonists, is reported. We used a highly potent serine protease inhibitor, Nafamostat, having an amidinonaphthyl unit as the starting compound. The compounds 4-(6-amidino-2-naphthylaminocarbonyl)phenoxyacetic acid (5a) and 4-(6-amidino-2-naphthalenecarboxamido)phenoxyacetic acid (5b) inhibited adenosin-5'-diphospate (ADP)-induced aggregation of human platelet-rich plasma (PRP) with IC50 values of 0.05 and 0.07 microM, respectively, and had lost their ability to inhibit a variety of serine proteases, including thrombin, factor Xa, plasmin and trypsin.     

一枝蒿酮酸苄酯类衍生物的合成、体外抗流感病毒和单纯I, II型疱疹病毒活性研究

为了提高一枝蒿酮酸的生物活性, 以一枝蒿酮酸和取代苄醇为原料. 在偶联剂DCC/DMAP的作用下, 合成了10种一枝蒿酮酸苄酯衍生物2a～2j, 所合成的化合物均经过IR, 1H NMR, ESI-MS等分析方法进行了表征, 并对所合成的化合物2a～2j进行了初步的体外抗A, B型流感病毒和单纯I, II型疱疹病毒活性研究, 结果表明: 大部分化合物对A, B型流感病毒具有较强的抑制活性, 其中化合物2e抑制A3, B型流感病毒的IC50值分别为5.5, 5.5 μmol/L, 化合物2i抑制A型流感病毒IC50值为: 7.8 μmol/L, 化合物2e和2i可作为抗流感病毒的先导化合物; 大部分化合物在0.1 μg/mL浓度下对I, II型疱疹病毒具有显著的抑制活性．     

Dmap-Catalyzed Synthesis of Novel Pyrrolo[2,3-D]Pyrimidine Derivatives Bearing an Aromatic Sulfonamide Moiety

4-(N,N-Dimethylamino)pyridine (DMAP), with a dual role as a basic nucleophilic catalyst, was shown to be a highly efficient catalyst for the synthesis of some new N-(2-aryl-7-benzyl-5,6-diphenyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)benzenesulfonamides through the reaction of 2-aryl-7-benzyl-5,6-diphenyl-7H-pyrrolo[2,3-d]pyrimidin-4-amines (7-deazaadenines) with benzenesulfonyl chlorides. It was also found that the use of DMAP under solvent-free conditions is much more effective than other catalytic systems such as pyridine as both the catalyst and solvent, t-BuOK in t-BuOH, Et₃N in ethanol (EtOH), and even DMAP in dimethylformamide (DMF). The influences of the reaction parameters, temperature, and the catalyst amount, on the catalytic performance have been studied. All synthetic compounds were characterized on the basis of their full spectral data.