3,5-二硝基苯甲酸淀粉酯的合成及应用

高分子吸附剂;3;5-二硝基苯甲酸淀粉酯的合成及应用     

纳米固体超强酸S2O2-8/ZrO2催化合成2-四氢呋喃甲酸冰片酯和2-四氢呋喃甲酸薄荷酯

以冰片、薄荷醇和2-四氢呋喃甲酸为原料,在纳米固体超强酸S2O2-8/ZrO2的催化下合成了2-四氢呋喃甲酸冰片酯和2-四氢呋喃甲酸薄荷酯,酯化率分别为67.6%和53.8%,其结构经NMR, IR和元素分析表征.     

(2,2-双二茂铁基丙烷)-6-甲酸酯的合成与表征

以2,2-双二茂铁基丙烷作为母体制得对应的甲酸,并以此合成了一系列未见文献报道的（2,2-双二茂铁基丙烷）-6．甲酸酯,其结构经1^H NMR,IR及元素分析表征。     

缬氨酸冰片酯合成及生物活性研究

本文从N-boc-L-缬氨酸和冰片出发,以DCC/DMAP作为催化剂合成了缬氨酸冰片酯(BPX),并采用IR、NMR、MS等方法对其结构进行了表征。进一步电休克惊厥实验及抑制HeLa细胞活力实验分别对缬氨酸冰片酯的抗癫痫及体外抑制肿瘤活性进行了初步研究,结果表明缬氨酸冰片酯显示出了明显的生物抗癫痫活性及抑制HeLa细胞增殖的能力。在最大电休克惊厥实验中,腹腔给药,当小鼠的BPX给药量为50mg·kg~(-1)及以上时,与对照组相比,显示出了与卡马西平类似甚至更好的抗癫痫活性;在体外抗肿瘤活性实验中,与对照组相比,BPX抑制率最高达57%,具备抑制HeLa细胞的增殖的能力。     

三烃基锡二茂铁甲酸酯的合成、表征及其生物活性

谱学表征;三烃基锡二茂铁甲酸酯的合成、表征及其生物活性     

三尖杉酯碱侧链酸的不对称合成及结构表征

以N-Boc苏氨醛为起始原料,经Wittig、Meisenheimer重排和催化氢化系列反应,不对称合成了天然产物三尖杉酯碱的侧链酸,中间体及目标产物结构经核磁共振(1 H NMR、13 C NMR)、红外光谱和质谱表征.结果表明,所用合成方法具有产率高、反应条件温和、操作简单等优点;目标化合物的总收率达30%.     

1,4-二氢-4-芳基-3,5-吡啶二羧酸酯的合成及表征

基于二氢吡啶化合物的构效关系, 设计了一系列1,4-二氢-4-芳基-3,5-吡啶二羧酸酯新化合物. 含有易于水解基团的1,4-二氢-4-芳基-3,5-吡啶二羧酸酯类化合物在碱性条件下水解合成了重要中间体1,4-二氢-4-芳基-3,5-吡啶二羧酸单酯, 收率93%～99.8%. 该二羧酸单酯与α-溴代芳基乙酮在相转移剂催化下反应合成目标化合物, 收率74%～99%. 中间体和目标化合物经¹H NMR, ¹³C NMR, IR, MS和元素分析等确证.     

纳米固体超强酸S_2O_8~(2-)催化合成正、异冰片酯的研究

以冰片、异冰片、乙酸、丙酸、丁酸、异丁酸为原料,首次采用纳米固体超强酸S2O28-/ZrO2催化合成了8个冰片、异冰片酯.酯化率42%～98%,反应选择性好,产物用1HNMR,13CNMR和IR进行结构确证.这些酯(除了乙酸冰片酯和乙酸异冰片酯外)的合成未见文献报道.     

季戊四醇螺环磷酸苯酚酯的合成及结构表征

季戊四醇螺环磷酸苯酚酯的合成及结构表征;季戊四醇螺环磷酸苯酚酯;季戊四醇螺环磷酰二氯;苯酚;绿色合成     

苯甲酸乙酯合成实验的改进

引入微波技术,对以硫酸为催化剂,水浴回流分水制备苯甲酸乙酯的传统方法进行合理改进,重点考察微波功率、反应温度、反应时间对产率的影响。采用正交设计安排实验,实验结果经过优化组合,得出最佳反应条件为：辐射时间15 min,微波功率600 W,反应温度95 ℃。利用微波辐射加热方式替代普通的沸水浴合成苯甲酸乙酯,达到缩短反应时间,提高反应效率的目的,产物用减压蒸馏分离纯化,整个实验教学具有绿色化、现代化和综合化的特点,有利于提高学生实验兴趣,同时保证了在有限的实验时间内有充足的知识点和充分的技能训练。     

Synthesis,Structure and Acaricidal Activity of Tricyclohexyltin Benzoate

Tricyclohexyltin 4-amino-3-methyl-benzoate(1) and tricyclohexyltin 3,4-dimethoxybenzoate(2) were synthesized and their crystal structures were determined by X-ray diffraction. Compound 1 belongs to the monoclinic system, space group P21/c with a = 14.0554(15), b = 11.6947(13), c = 16.2720(17) , Z = 4, V = 2565.7(5) 3, Dc = 1.341 g·cm-3, μ(MoKα) = 1.016 mm-1, F(000) = 1080, R = 0.0833 and wR = 0.2964. Compound 2 is of monoclinic system, space group C2/c with a = 17.8712(6), b = 8.4433(3), c = 35.5783(13) , Z = 8, V = 5366.8(3) 3, Dc = 1.360 g·cm-3, μ(MoKα) = 0.980 mm-1, F(000) = 2288, R = 0.0549, wR = 0.1279. In compounds 1 and 2, the central Sn atom is coordinated in a tetradentate manner to assume a distorted tetrahedral configuration. Preliminary biological tests showed that these two compounds have strong acaricidal activity.     

Synthesis and Crystal Structure of Tetra Benzoates Bridged Binuclear Sm(III) Complex

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Synthesis, Crystal Structure and Thermal Stability of a Saturated Dimeric Ce(III)-chelated Complex Based on Benzoate and 1,10-Phenanthroline Ligands

The title complex, [Ce(BA)3phen]2 (BA = benzoate, phen = 1,10-phenanthroline), was prepared by the reaction of Ce(NO3)3·6H2O, benzoic acid and 1,10-phenanthroline. The complex was characterized by single-crystal X-ray diffraction, elemental analysis, IR spectra and TG-DTG techniques. The results show that the crystal is of triclinic, space group P1 with a = 10.912(2), b = 11.962(3), c = 12.474(3) , α = 104.889(3), β = 93.523(3), γ = 113.332(3)o, C66H46Ce2N4O12, Mr = 1366.90, V = 1420.2(6) 3, Z = 1, Dc = 1.598 g/cm3, μ = 1.652 mm-1, S = 1.024 and F(000) = 682. The final R = 0.0391 and wR = 0.0947 for 4878 observed reflections with I > 2σ(I). The structure of the title complex consists of two Ce(C6H5COO)3(C12H8N2) units, forming a binuclear molecule. Each Ce(III) is coordinated by two O atoms of one bidentate chelating carboxylate group, five O atoms of two bidentate bridging and two tridentate chelating-bridging carboxylate groups, and two N atoms of one 1,10-phenanthroline molecule to complete a distorted monocapped square antiprism geometry. Its thermogravimetric analysis was determined by TG-DTG techniques.     

Synthesis and Crystal Structure of Glycin·3,5-Dihydroxybenzoic Acid

The title compound glycin·3,5-dihydroxybenzoic acid (GDB) has been synthesized and characterized by single-crystal X-ray analysis. It crystallizes in orthorhombic, space group Pca21 with a = 25.513(10), b = 4.668(2), c = 9.150(4)(A), Z = 4, V = 1089.8(8)(A)3, C9H13NO7, Mr = 247.20, Dc = 1.507 g/m3, μ(MoKα) = 0.132 mm-1, F(000) = 520, R1 = 0.0322 and wR2 = 0.0611 for 885 observed reflections (I > 2σ(I)). The title compound is a 1:1 molecular complex of glycin and 3,5-dihydroxybenzoic acid, which is linked by O-H…O and N-H…O hydrogen bonds to form a three-dimensional framework. Test of SHG (second harmonic generation) indicates that NLO generation of the crystal is higher than that of KDP.     

Synthesis and Crystal Structure of 3,5-Dichloro-N-(2-methoxyphenyl)benzamide

<正>The title compound was synthesized by the direct reaction of 3,5-dichlorobenzoic acid with 2-methoxyaniline in the presence of DCC and HOBT. The structure was supported by the spectroscopic data and unambiguously confirmed by the single-crystal X-ray diffraction studies. It crystallizes from a methanol solution in the monoclinic space group P2_1/c with unit cell dimensions of a = 4.9369(16), b = 13.351(5), c = 20.168(7), β = 96.755(8)°, V = 1320.1(8)~3 and Z = 4.     

2,6-二氨基-3,5-二硝基吡嗪-1-氧化物的合成及其晶体结构

以三氟乙酸为溶剂和催化剂,2,6-二氨基-3,5-二硝基吡嗪与过氧化氢反应制备了2,6-二氨基-3,5-二硝基吡嗪-1-氧化物(LLM-105),其结构经1H NMR,IR,MS,元素分析和四圆单晶X-射线衍射仪表征。LLM-105属单斜晶系,空间群P21/n,晶胞参数:a=0.571 6(3)nm,b=1.593 5(5)nm,c=0.841 2(5)nm,α=90°,β=100.97(4)°,γ=90°,V=0.7522(6)nm3,Dc=1.908 g.cm-3,Z=4,μ=0.175 mm-1,F(000)=440,μ(MoKα)=1.047 mm-1;R1=0.053 2,wR2=0.137 9。LLM-105存在分子内和分子间氢键。     

固载杂多酸盐催化合成苯甲酸正戊酯

首次报道了以固载杂多酸盐TiSiW12 O4 0 /TiO2 为多相催化剂 ,对以苯甲酸和正戊醇为原料合成苯甲酸正戊酯的反应条件进行了研究 .实验表明 :TiSiW12 O4 0 /TiO2 是合成苯甲酸正戊酯的良好催化剂 .最佳反应条件为 :醇酸物质量比为 4∶1,催化剂用量为反应物料总量的 1.5 % ,反应时间为 2 .5h .上述条件下 ,苯甲酸正戊酯的产率可达 96 .7% .     

层状氢氧化苯甲酸锌的水热合成与表征

在110～180 ℃范围内, 以Zn(OH)2与苯甲酸为原料水热法成功合成了层状氢氧化苯甲酸锌化合物. 通过XRD、TG-DTA、SEM、TEM和元素分析研究了合成产物的结构、形貌、性质和化学组成, 探讨了合成条件对水热反应产物的影响. 当C6H5COOH/Zn的摩尔比为0.9～1.0, 水热温度130～150 ℃及水热反应12 h, 合成的层状化合物具有纤维状粒子特征, 层间距为1.44 nm, 化学组成为Zn(OH)1.12•(C6H5COO)0.88.