两种新型抗癌药的结构鉴定

本文应用质谱、核磁共振波谱、红外光谱及元素分析等方法对1-(2-四氢呋喃)-5-氟脲嘧啶(FT-207)和1,3-双(2-四氢呋喃)-5-氟脲嘧啶(FD-1)两种新型抗癌药进行了结构鉴定。     

新型5-苯亚甲基-3,4-二卤-2(5H)-呋喃酮衍生物的合成与生物活性

以粘卤酸为起始原料,经还原缩合、再缩合、成醚反应合成了15个5-苯亚甲基-3,4-二卤-2(5H)-呋喃酮衍生物4a-4o,其结构经~1H-NMR、~(13)C-NMR、MS谱确证.研究所有化合物对细菌脂多糖LPS诱导RAW264.7细胞的抗炎作用.初步活性结果显示,4a-4o对于LPS诱导RAW264.7细胞所产生的NO有抑制作用,其中化合物4h和4i的NO抑制率比较高.生物活性的研究结果表明,卤代呋喃酮结构、吡啶环上连有给电子基团都可以提高化合物的体外抗炎生物活性,为临床上炎症等相关疾病的治疗提供新的药物设计和研究思路.     

机械研磨法合成5-(2-硝基烷基)米氏酸衍生物

以5-亚烃基米氏酸衍生物与硝基烷烃类化合物在固相机械研磨条件下,在碱存在下,反应合成5-(2-硝基烷基)米氏酸衍生物,探讨了碱、反应物料比等条件对产物产率的影响,优化反应条件为:等物质的量的甲醇钠,反应温度50℃,反应时间30 min.该方法适用于合成多种5-(2-硝基烷基)米氏酸衍生物,为γ-氨基丁酸衍生物的合成提供...     

新型5-HT重摄取抑制剂的设计、合成及活性评价

在对已知各种结构类型的5-HT重摄取抑制剂分子结构全面分析的基础上, 建立了SSRIs药效团模型. 基于该模型应用UNITY程序对NCI-3D和Maybridge-3D数据库进行三维结构的限制性查询, 在获得的命中结构的信息指导下, 设计合成了3种全新结构类型的化合物, 并完成了初步的药理活性评价. 这些化合物均显示出不同程度的5-HT重摄取抑制活性, 其中5个化合物显示高抑制活性. 哌嗪取代的二苯脒类化合物的结构新颖, 较好地符合5-HT重摄取抑制剂药效团模型, 与SSRIs类化合物三维定量构效关系研究得到的CoMFA模型有较好的适配性.     

一种新型疏水改性的两亲性壳聚糖衍生物的表面活性研究

鉴于甲壳质的生物降解性、生物活性和生物相容性等诸多特性 ,其开发利用正受到人们的广泛重视[1] .具有不同性能和功效的衍生物已在医药、食品、日用化工、纺织、水处理等领域发挥了重要的作用 [2～ 4 ] .然而具有表面活性的两亲性衍生物却少见报道 [5,6] .本文将羧甲基壳聚糖进行疏水改性 ,使其分子上同时具有亲水基和疏水基 ,从而具有两亲性质 ,可以降低溶液的表面张力 ,并在溶液中形成胶束 .可望在日用化工、医药、食品等领域起到降低表面张力、增稠、乳化和增溶等作用 .1　实验部分1 .1　原料及仪器　羧甲基壳聚糖 (CMCHS,青岛生化制…     

含手性的胺类冰片衍生物的合成

含氮类化合物在自然界中广泛存在,且大多具有生物活性,并且与人体的健康有着密切的关系。在含氮类化合物中,胺类及其衍生物是十分重要的,它们在有机反应中是有用的中间体,同时,它们还存在于很多生物体中。因此,对胺类及其衍生物的研究很有意义。2(5H)-呋喃酮作为一个结构组分广     

一种新型卟啉-脂质体衍生物的合成及表征

采用人工合成的N,N-二.十六烷基-6-溴代-L-甘氨酰胺(BrC5Gly2C16H33)与5,10,15-三苯基-20-对羟基苯基卟啉(HPTPP)相连接,合成了一种新型卟啉-脂质体衍生物(P-L),用元素分析、紫外可见光谱、核磁共振、红外光谱以及荧光光谱等方法进行了表征,并对其谱学性质进行了研究.     

一种新型锰MOF的合成、结构和磁性的研究

通过水热合成法以1-(4羧苯基)-1H-苯并咪唑-5,6-二羧酸为配体合成了一种新型金属锰MOF[Mn(Hcbic)]n(H3cbic=1-(4羧苯基)-1H-苯并咪唑-5,6-二羧酸),并通过X-ray进行了单晶分析.该Mn-MOF是包含了一维左、右双螺旋链,螺距约为0.3902 nm,同时配体Hcbic2-中的4-...     

新喜树碱衍生物的核磁共振谱分析与结构鉴定

以20(S)-喜树碱(CPT)为起始原料,对其进行结构修饰,合成了一种新的喜树碱衍生物CPT-A.并利用1D(~1H、~(13)C和DEPT135)和2D(异核单量子相关谱和异核多碳相关谱)核磁共振(NMR)技术对该化合物进行了结构确定,详细归属了CPT-A~1H和~(13)C NMR谱的化学位移,喜树碱骨架的指认结果与文献报道基本一致,并发现喜树碱骨架6位碳与取代基苯环3’位碳的化学位移相同,谱峰完全重叠,这在~(13)C谱中是不常见的.研究结果可为喜树碱类天然产物的发现和结构鉴定提供NMR数据支持和方法指引.     

具有酰基或氨基甲酰基结构的5-氟尿嘧啶衍生物的合成及抗肿瘤活性

5-氟尿嘧啶(5-FU)首先由 Duschinsky 和Pleven 合成。作为一种广谱性的抗肿瘤临床药物,其主要缺点是脂溶性小,口服吸收困     

Synthesis,Crystal Structure and Biological Activity of a New 4,5-Diaryl-lH-imidazole Derivative

A new 4,5-diaryl-lH-imidazole was synthesized and characterized by 1H NMR, ESI-MS, elemental analysis and FT-IR. The crystal structure of the title compound （C19H16C12N202, Mr = 375.24） has been determined by single-crystal X-ray diffraction. Crystal parameters： mono- clinic system, space group P2/n, a = 14.349（3）, b = 8.7918（18）, c = 15.352（3） A, β = 108.56（3）°, V = 1836.1（6） A3, Z = 4, F（000） = 776, Dc = 1.357 g/cm3, p = 0.368 mm-1, the final R = 0.0502 and wR = 0.1066 for 2324 observed reflections with 1 〉 2 σ（/）. A total of 16117 reflections were collected, of which 3615 were independent （Rint = 0.0595）. The preliminary bioassay suggested that the title compound exhibits distinct effective inhibition on the proliferation of cancer cell lines.     

Synthesis,Structure,Characterization and Electrochemistry of a New Din

Reaction of Et4NCl, NaSCH2COOMe and W(CO)6 in MeCN affords a new dinuclear tungsten(0) complex [Et4N]2[W2(CO)8(SCH2COOMe)2] (1). The crystal and molecular structure has been determined by X-ray single crystal diffraction. 1 Crystallized in the triclinic, space group P with a=11.141(7), b=10.267(4), c=10.798(3)(); α=93.96(3), β=96.88(4), γ=114.97(5)°; V=1003()3, Z=1, Dc=1.76 g/cm3, μ=60.1 cm-1, R=0.042 and Rw=0.050 for 2967 independent reflections with I>3.0 σ(I). 1 contains a WS2W planar core with nonbonding W...W distance of 3.9611(5)(), and its IR, 13C NMR, and cyclic voltammetry were measured and discussed.     

Synthesis and Crystal Structure of a New Adamantane Amide Derivative

A novel adamantane acyl amide derivative containing two phthalimido pendant groups(C31H31N3O5) has been synthesized,and its structure was characterized by elemental analysis,IR,1 H NMR spectra,and single-crystal X-ray diffraction.The crystal belongs to triclinic,space group P1 with a=7.3158(10),b=13.2405(18),c=14.378(2),α=72.419(2),β=84.496(2),γ=81.799(2)o,V=1312.0(3)3,Z=2,Dc=1.330 g/cm 3,μ=0.09 mm-1,Mr=525.59,F(000)=556,S=1.001,R=0.0523 and wR=0.0707 for 5901 unique reflections with 2363 observed ones(I>2σ(I)).π-π stacking interactions(offset face-to-face) exist between the two rings of phthalimides from the neighboring molecules in the title crystal structure.The intermolecular dihedral angle between the two rings of neighboring phthalic amides is 6.26° and the distance is 4.008.     

Discovery of a Prenylated Flavonol Derivative as a Pin1 Inhibitor to Suppress Hepatocellular Carcinoma by Modulating MicroRNA Biogenesis

Peptidyl‐prolyl cis‐trans isomerase Pin1 plays a crucial role in the development of human cancers. Recently, we have disclosed that Pin1 regulates the biogenesis of miRNA, which is aberrantly expressed in HCC and promotes HCC progression, indicating the therapeutic role of Pin1 in HCC therapy. Here, 7‐(benzyloxy)‐3,5‐dihydroxy‐2‐(4‐methoxyphenyl)‐8‐(3‐methylbut‐2‐en‐1‐yl)‐4H‐chromen‐4‐one ( AF‐39 ) was identified as a novel Pin1 inhibitor. Biochemical tests indicate that AF‐39 potently inhibits Pin1 activity with an IC₅₀ values of 1.008 μm , and also displays high selectivity for Pin1 among peptidyl prolyl isomerases. Furthermore, AF‐39 significantly suppresses cell proliferation of HCC cells in a dose‐ and time‐dependent manner. Mechanistically, AF‐39 regulates the subcellular distribution of XPO5 and increases miRNAs biogenesis in HCC cells. This work provides a promising lead compound for HCC treatment, highlighting the therapeutic potential of miRNA‐based therapy against human cancer.     

一种乳酸菌胞外多糖糖链结构解析

以分离纯化得到的一种嗜热链球菌分泌的胞外多糖EPS03-1gm为研究对象, 采用气相色谱、分光光度及核磁共振技术对该多糖重复单位结构进行了解析. 结果表明, EPS03-1gm的单糖组成是葡萄糖和半乳糖, 不含糖醛酸和蛋白成分, 其重复单位中有4个糖基单元且都是6C糖. DEPT谱说明每个重复单位中有4个CH2, 用二维核磁共振谱和HMQC及HMBC谱分别对4个糖单元中的H和C进行了归属. 确定该多糖重复单位的糖链结构为: →3)-α-D-Galp-(1→3)-β-D-Galf-(1→3)-β-D-Glcp-(1→6)-β-D-Glcp-(1→.     

Synthesis and Structure of Tetrahydro-4,7-ethanoisobenzofuran-1,3-dione Derivative

(1R,2R,3S,4R,7R)‐7‐Isopropyl‐6‐methylbicyclo[2.2.2]oct‐5‐ene‐2,3‐dicarboxylic acid anhydride (tetrahydro‐4,7‐ethanoisobenzofuran‐1,3‐dione derivative) adduct 2 was prepared via the isomerization of α‐pinene and β‐pinene in turpentine followed by the Diels‐Alder cycloaddition with maleic anhydride in the presence of phosphoric acid/iodine catalysis. The molecular structure of adduct 2 was characterized by IR, ¹H NMR, ¹³C NMR, ¹H‐¹H COSY, DEPT, HSQC, HMBC, 2D NOESY and MS spectra. The single crystal X‐ray crystallographic analysis of adduct 2 was performed, and the X‐ray powder diffractive spectrum of the sample adduct 2 is consistent with the diffractive spectrum calculated from the single crystal data. Therefore the structure and stereochemistry of adduct 2 was established based on extensive spectral data and single crystal X‐ray analysis.     

1,5-苯并硫氮杂-α-苯基-β-内酰胺的合成及晶体结构

1，5-苯并硫氮杂与苯乙酰氯反应生成1，5-苯并硫氮杂-α-苯基-β-内酰胺（Ⅱ）。X-射线单晶衍射测定结果表明，该化合物分子式为C29H22CINOS，M=467.5，晶体属单斜晶系，P21／c空间群，a＝12．864（3），b=9．511（2），c=19．489（4）A，β=92.41（3）°，V=2382（1）A3，Dc=1．305g／cm3，Z=4，F（000）=976，μ=0．2636mm－1，R=0．068，Rw=0.068。该反应具有立体专一性，四员环上的2个苯基位于同一侧为顺式。产物分子中的七员环为类椅式构象。     

高硅ZSM-5分子筛和二次合成Ti-ZSM-5分子筛的结构

运用度角旋转（MAS）和交叉极化（CP）等核磁共振波谱和红外光谱技术，分别对采用不同模板剂制备的高硅ZSM－5分子筛和以此为母体，经气固同晶取代法得到Ti－ZSM－5分子筛的结构特性进行了研究．结果表明：在水热法合成高硅ZSM-5分子筛过程中，模板剂明显制约着所制得的分子筛的结构特性．通过选用合适的模板剂，可直接获得具有正交晶系结构的高硅ZSM－5分子筛．在随后的气固相同晶取代过程中，钛原子通过占据分子筛骨架中的缺陷位进入骨架，形成具有一定Ti／Si比例的钛硅分子筛（Ti－ZSM－5）。骨架结构中缺陷位的含量直接影响分子筛的载钛量。     

Synthesis,Crystal Structure and Cytotoxic Activity of a New NAN-190 Analogue

The NAN-190 analogue 2-(2-(2-(4-(2-methoxyphenyl)piperazin-1-yl)ethoxy)ethyl)isoindoline-1,3-dione(1, C23H27N3O4, Mr = 409.48) was synthesized via a three-step reaction and characterized by 1H NMR, 13 C NMR, ESIMS and single-crystal X-ray diffraction. The crystal belongs to orthorhombic, space group Pna21 with a = 7.6445(15), b = 38.851(8), c = 7.1316(14) A, V = 2118.0(7) A3, Z = 4, Dc = 1.2840 mg/mm3, μ = 0.089 mm-1, F(000) = 872.4, R = 0.0545 and w R = 0.1681. The single-crystal X-ray structural analysis reveals that the piperazine ring in compound 1 presents a stable and minimum energy chair conformation. In addition, the preliminary cytotoxic assay shows that the title compound exhibits strong and selective inhibitory activity against DU145 cells(IC50 = 5.88 ± 1.02 μM).