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1.
前已报道葫芦科(Cucurbitaceae)植物假贝母(Bolbostemma paniculatum [Maxim]Franquet)鳞茎土贝母中四个三萜皂苷土贝母苷甲、乙、丙、丁的提取与分离以及土贝母苷甲的结构研究.本文继续报道其余三个皂苷的结构研究. 土贝母苷乙(1),白色粉末,C_(63)H_(98)O_(30),[α]_D—6.0(c0.32,吡啶),M_r1334(SIMS: m/(?)1335[M+H]~+).苷元为远志酸(2),所含的糖为葡萄糖、鼠李糖、阿拉伯糖和木糖,摩尔比为1:1:2:1.1的~(13)C NMR谱中显示五个糖端基碳信号(δ106.4,104.8,103.2,100.8和94.3  相似文献   

2.
从葫芦科植物假贝母(Bolbostemma paniculatum[Maxim] Franquet)的鳞茎中分得五个苷类化合物:土贝母苷甲(1)、乙、丙、丁和戊.通过对1及其各选择性水解产物的 NMR 分析确定了它的结构,为一新的三萜皂苷.  相似文献   

3.
土贝母化学成分的研究 IV: 土贝母苷乙, 丙, 丁的结构   总被引:5,自引:0,他引:5  
从葫芦科(Cucurbitaceae)植物假贝母(Bolbostemma paniculatum [Maxin]Franquet)鳞茎中分离到三个土贝母苷乙, 丙, 丁. 用光谱分析和化学降解鉴定了它们的结构, 土贝母乙, 丙是二个新的大环三萜皂苷, 土贝母丁是3-O-[α-L-吡喃阿拉伯糖基(1→2)-β-D-吡喃葡糖基]-3β, β-18, 20, 26-五羟-(20S)-达马-24-烯, 是从植物假贝母中分离到的仅有四环三萜.  相似文献   

4.
人血清白蛋白多种结合位点的存在使其成为许多药物可能的结合靶点.土贝母皂苷具有广泛的生理和药理活性,它与蛋白质相互作用机制的研究对于深入了解其药理药效具有重要的意义.采用荧光光谱法研究了土贝母皂苷II(TBMSⅡ)与人血清白蛋白(HSA)之间的相互作用,根据Stern-Volmer荧光淬灭方程计算得293,298,303...  相似文献   

5.
在检测中药材黄芪中黄芪甲苷含量时,将高效液相色谱的二极管阵列检测器和蒸发光散射检测器串联使用,并结合光谱和质谱分析技术,对黄芪甲苷的伴生组分进行了研究.结果表明,不同产地的黄芪样品中,黄芪甲苷的含量差别较大,其伴生组分的种类和含量也有很大不同.此项研究对于深入评估黄芪的品质具有一定的参考价值.  相似文献   

6.
宋凤瑞  闫存玉  刘宁  刘志强  刘淑莹 《分析化学》2005,33(12):1743-1746
选择与SAPS病毒相关的DNA片段作为抗病毒药物筛选的靶分子,利用生物质谱技术,通过对该寡聚去氧核苷酸分子与常见中药黄芪、穿心莲、刺五加、苦杏仁、牛蒡子、栀子、菘蓝(板蓝根、大青叶)及厚朴中的主要化学成分——黄芪甲苷、苦杏仁苷、穿心莲内酯、栀子苷、紫丁香苷、牛蒡子苷、靛蓝、靛玉红、厚朴酚及和厚朴酚的相互作用研究,发现与寡聚去氧核苷酸的作用强度顺序为:黄芪甲苷>苦杏仁苷>穿心莲内酯>栀子苷>紫丁香苷>牛蒡子苷、靛玉红、靛蓝、厚扑酚及和厚朴酚与寡聚去氧核苷酸没有复合物形成。还研究了黄芪甲苷与3种脱氧核苷的相互作用。本方法作为药物筛选具有一定的可行性。  相似文献   

7.
核糖在酸的作用下于甲醇中闭环得到呋喃核糖甲苷,将其2,3-二羟基形成异亚丙基后,与对甲苯磺酰氯作用生成5-O-对甲苯磺酰基-2,3-O-异亚丙基-1-α/β-D-呋喃核糖甲苷,最后与取代哌嗪或吗啉反应,再在酸的作用下除去2,3-保护基,得到5-脱氧-5-杂环取代-1-α/β-D-呋喃核糖甲苷.它们的结构经~1H NMR和MS确证.  相似文献   

8.
陈力  梁芬芬  许美凤  邢国文  邓志威 《化学学报》2009,67(12):1355-1362
详细研究了N-乙酰基-5-N,4-O-噁唑烷酮保护的唾液酸对甲基苯硫苷给体1与四种苄基或苯甲酰基保护的半乳糖甲苷二醇的唾液酸化反应, 以较高的产率(72%~89%)得到了相应的唾液酸化产物, α/β=(1.6~2.0)∶1. 在此基础上, 以乳糖为原料通过7步反应以19%的总产率制得了2,3,6,2’,6’-五-O-苯甲酰基-β-乳糖甲苷17, 使用唾液酸给体1将化合物17唾液酸化, 成功地得到神经节苷脂GM3三糖甲苷衍生物18, 产率68%, α/β=1.6∶1.  相似文献   

9.
采用2,2,6,6-四甲基哌啶氧自由基/Ca(ClO)2体系选择氧化甲基葡萄糖苷(简称甲苷)合成了葡萄糖甲苷酸盐,再用硫酸酸解葡萄糖甲苷酸盐,得到葡萄糖醛酸和副产物硫酸钙。考察了氧化工艺条件对葡萄糖醛酸收率的影响;用pH计监控反应过程,反应中间体和终产物用UV和HPLC检测。结果表明,该体系对甲苷伯羟基的氧化具有较好的催化活性和反应选择性,葡萄糖醛酸收率达到92%,且金属离子易于去除。和传统的淀粉HNO3氧化法工艺相比,该方法具有资源节约、环境友好的特点。  相似文献   

10.
以3,5-二硝基苯甲酰氯为衍生化试剂,柱前衍生,ODS2柱分离,V(甲醇):V(0.01 mol/L KH2PO4)=60:40(H3PO4调节pH 3.5)洗脱,紫外(230 am)检测,建立了黄芪甲苷的反相高效液相色谱法.在5.0~100 μg/mL范围内,黄芪甲苷的峰面积与其浓度呈现良好的线性关系.回归方程为A=478944+2132c,相关系数为0.9986.相对标准偏差为2.7%(c=20.0 μg/mL,n=6),加标回收率在97.8%~103.4%.该法已用于黄芪中黄芪甲苷含量的测定.  相似文献   

11.
X-ray photoelectron spectroscopy (XPS) along with inductively coupled plasma analysis (ICP-AE) and Raman spectroscopy have been used to define the location and to quantify the amount of iodine in HiPco SWNT samples loaded with molecular I(2) via sublimation (I(2)-SWNTs). The exterior-adsorbed I(2) can be removed (as I(-)) by reducing the sample of filled nanotubes with Na(0)/THF or by heating the I(2)-SWNTs to 300 degrees C (without reduction), leaving I(2) contained only within the interior of the SWNTs (I(2)@SWNTs) as proven by XPS. These I(2)@SWNTs contain approximately 25 wt % of I(2) and are stable without the loss of I(2) even after exposure to additional reduction with Na(0)/THF or upon heating to ca. 500 degrees C.  相似文献   

12.
A new Cs(I) magnetic ion-imprinted polymer (Cs(I)-MIIP) aimed at the selective adsorption and separation of Cs(I) from salt lake brine was prepared. The Fe3O4@SiO2 was used as supporter, Cs(I) as template ion, and carboxymethyl chitosan as functional monomer. The product was characterized by Fourier transform infrared spectra, XRD, energy-dispersive spectrometry, scanning electron microcopy, thermogravimetric analysis, and vibrating sample magnetometer. The adsorption of the Cs(I)-MIIP in solution was investigated, which indicated the maximum adsorption capacity was 36.15?mg·g?1 under the optimum conditions. The pseudo-first-order kinetic model and the Freundlich isotherm model were applied to predict the adsorption process of Cs(I) onto Cs(I)-MIIP. Selectivity experiments showed that the relative selectivity coefficient (k′) were 24.995, 1.73, 1.43, 4.83, and 1.63 to Cs(I)/Li(I), Cs(I)/Na(I), Cs(I)/K(I), Cs(I)/Rb(I), and Cs(I)/Sr(II) binary solutions, higher than those of NIP, respectively. Furthermore, the Cs(I)-MIIP was successfully applied to the enrichment and separation of Cs(I) from the salt lake brine of Qinghai, with satisfactory Cs(I) recovery rates.  相似文献   

13.
2-取代苯亚胺基噻唑烷类化合物的晶体结构研究   总被引:2,自引:0,他引:2  
A series of 2-phenyliminothiazolidines has been successfully synthesized; and 2-(2-methylphenyl) iminothiazolidine (I a) and 2-(4-methylphenyl) iminothiazolidine (I b) have been selected to determine their crystal structures by X-ray diffraction technique,from their molecular graph of it is shown that double bond at 2-carbon atom of the heterocycle is all extro-cychc at the crystal state,and there are two main plaines in I a and I b.But in I a ,the angle between the planes is 61.4° and in I b the angle is about 41.4°.And so there is a strong conjugative effect in I b than in I a.So it is thought that the difference in fungicidal activities between 2-substitutedphenyl compounds (I a) and 4-substitutedphenyl compounds(I b) is due to their space factors.  相似文献   

14.
Lehn JS  Hoffman DM 《Inorganic chemistry》2002,41(15):4063-4067
Zirconium amide-iodide complexes were synthesized for possible use as chemical vapor deposition precursors to zirconium nitride films. The series of six complexes Zr(NR(2))(4-n)I(n)(R = Me or Et; n = 1-3) was prepared by reacting ZrI(4) and Zr(NR(2))(4) in hot toluene. X-ray crystallographic analyses were performed for Zr(NMe(2))(3)I, Zr(NEt(2))(2)I(2), and Zr(NEt(2))I(3). In the solid state, Zr(NMe(2))(3)I and Zr(NEt(2))(2)I(2) are the discrete dimers [Zr(NMe(2))(2)I(mu-NMe(2))](2) and [Zr(NEt(2))(2)I(mu-I)](2), and Zr(NEt(2))I(3) is the polymer of dimers ([Zr(NEt(2))I(2)(mu-I)](2))(n). In solution, Zr(NEt(2))(3)I is proposed to be monomeric on the basis of NMR data and a molecular weight determination. The complex Zr(NEt(2))(3)I is the most promising precursor candidate because of its physical properties.  相似文献   

15.
The formation of high-n Rydberg atoms from the neutral dissociation of superexcited states of I(2) formed by resonant two-photon excitation of molecular iodine using an ArF laser has been investigated. The high-n Rydberg atoms I* are formed by predissociation of the optically excited molecular Rydberg states I*(2)[R(B (2)Sigma(g) (+))] converging on the I(2) (+)(B (2)Sigma(g) (+)) state of the ion. Measurement of the kinetic energy release of the Rydberg I* fragments allowed the identification of the asymptotic channels as I*[R((3)P(J))]+I((2)P(32)), where the I*[R((3)P(J))] are Rydberg atoms converging on the I(+)((3)P(J)) states of the ion with J=2, 1, and 0. In the case of the I*[R((3)P(2))] fragments, the average Rydberg lifetime is observed to be 325+/-25 micros. Based on experiments on the variation of the Rydberg atom signal with the field ionizing strength, the distribution of Rydberg levels peaks at about 25-50 cm(-1) below the ionization limit.  相似文献   

16.
Photoelectron spectra and angular distributions in 267 nm detachment of the I(-)Ar, I(-)H(2)O, I(-)CH(3)I, and I(-)CH(3)CN cluster anions are examined in comparison with bare I(-) using velocity-map photoelectron imaging. In all cases, features are observed that correlate to two channels producing either I((2)P(3/2)) or I((2)P(1/2)). In the photodetachment of I(-) and I(-)Ar, the branching ratios of the (2)P(1/2) and (2)P(3/2) channels are observed to be approximately 0.4, in both cases falling short of the statistical ratio of 0.5. For I(-)H(2)O and I(-)CH(3)I, the (2)P(1/2) to (2)P(3/2) branching ratios are greater by a factor of 1.6 compared to the bare iodide case. The relative enhancement of the (2)P(1/2) channel is attributed to dipole effects on the final-state continuum wave function in the presence of polar solvents. For I(-)CH(3)CN the (2)P(1/2) to (2)P(3/2) ratio falls again, most likely due to the proximity of the detachment threshold in the excited spin-orbit channel. The photoelectron angular distributions in the photodetachment of I(-), I(-)Ar, I(-)H(2)O, and I(-)CH(3)CN are understood within the framework of direct detachment from I(-). Hence, the corresponding anisotropy parameters are modeled using variants of the Cooper-Zare central-potential model for atomic-anion photodetachment. In contrast, I(-)CH(3)I yields nearly isotropic photoelectron angular distributions in both detachment channels. The implications of this anomalous behavior are discussed with reference to alternative mechanisms, affording the solvent molecule an active role in the electron ejection process.  相似文献   

17.
结合共振增强多光子电离(REMPI)方案,利用离子影像技术研究了n-C3H7I和i-C3H7I分子的光解动力学.分析和比较了它们光解过程中所涉及的能量分配和解离态间的非绝热跃迁信息.它们的I(2P3/2)产物通道的内能所占百分比要大于I*(2P1/2)产物通道的.随着烷烃自由基变得更加的分支化,一方面,原子碎片(I和I*)的能量分布明显变宽,暗示了α-碳原子上的烷基具有更复杂的振转模式;另一方面,在266nm光子的泵浦下,尽管两分子3Q0邝X跃迁的谐振强度表现出很小的差别,但是,产生I*碎片的几率明显降低,从n-C3H7I的0.72降到i-C3H7I的0.46.这可以归因于在光解i-C3H7I过程中弯曲振动模式对产生I和I*的贡献要比n-C3H7I光解过程中弯曲振动模式对I和I*的贡献更明显,使得3Q0与1Q1态之间的非绝热跃迁得到增强.此外,n-C3H7I和i-C3H7I的3Q0邝X跃迁并不完全是平行跃迁,对应的跃迁偶极矩与键轴间的夹角分别约为15°和18°.  相似文献   

18.
The kinetics of activation of RX by a Cu(I) complex has been investigated in MeCN both in the absence and presence of halide ions. The system Cu(I)/L/X(-) (L = Me(6)TREN) is mainly composed of Cu(I)L(+), XCu(I)L and Cu(I)X(2)(-), but only Cu(I)L(+) is found to be an active catalyst reacting with RX.  相似文献   

19.
Crystal and molecular structure of μ-oxo-bis[trifluoroacetato(p-tolyl)iodine] (I) synthesized by a new procedure was determined by X-ray diffraction analysis. Crystals I are orthorhombic, unstable, space group Pbcn, a=17.684(3), b=8.453(3), c=30.560(4) Å, Z=8. The structure of I was solved by direct and Fourier methods and refined by the full-matrix least-squares procedure in an anisotropic-isotropic approximation to R=0.098 (CAD-4 automatic diffractometer, λCuKα, 1200 observed reflections with I≥2σ). In molecule I, two iodine atoms have T-configuration of valence bonds with the average bond angles O?I?O 169(1) and O?I?C 86(2)°, average bond lengths I?Oμ 2.009(9), I?Oacet 2.269(9), and I?Caryl 2.11(1) Å, and the bond angle I?O?I 118.1(5)°. In molecule I, two p-Tol substituents are directed to approximately the same side of the medium plane of the central O?I?O?I?O fragment. Crystal structure I has I...O type intra-and intermolecular nonvalent interactions (secondary bonds).  相似文献   

20.
The S-R enantiomerization processes of 2,2'-biphenol (biphenol) have been investigated using density functional theory (DFT). Five isomers for biphenol were identified: I0, which is the most stable isomer; I1a and I1b, which are formed by a restricted rotation of one OH group; and I2a and I2b, which are formed by a restricted rotation of the two OH groups where a and b denote cis and trans configurations, respectively. Each isomer has R- and S-enantiomers. The energies relative to the most stable isomer I0 are 1.6, 3.3, 5.3, and 5.5 kcal mol(-1) for I1a, I1b, I2a, and I2b, respectively. The direct enantiomerization of I0, in which the phenol-ring rotation is considered to be the reaction coordinate while the OH rotations are frozen, is forbidden because of the repulsion between the two OH groups. The transition states for isomerizations of I0 to other isomers (I1a, I1b, I2a, or I2b) were calculated as well as those for the other direct enantiomerizations except for that of I0. From the viewpoint of the least number of the transition states and their low energy levels, the probable S-R enantiomerization of I0 is expressed as a sequential process of isomerization: I0,S --> I1a,S, a direct enantiomerization induced by one of the two OH rotations, I1a,S --> I1a,R, and another isomerization, I1a,R --> I0,R, that is, I0,S --> I1a,S --> I1a,R --> I0,R as the whole process. This process is effective in quantum control of the enantiomerization of biphenol and can be carried out by a sequence of a pump-dump IR laser-pulse scheme.  相似文献   

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