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61.
A modified poly(ethylene glycol) (PEG) has been developed as the soluble polymeric supports for liquid phase synthesis of novel thiourea derivatives.In each step of the sequence,the PEG-bound products were precipitated in cold Et2O and the unreacted materials and by-products were removed by simple filtration.The progress of reaction,purity of the isolation and the structure of the PEG-bound products were easily monitored by TLC,IR and ^1H NMR spectra.Representative thiourea derivatives were obtained in moderate yields with excellent purity from this modified PEG-bound product by the cleavage with 50% TFA/H2O. 相似文献
62.
两亲性丙烯酸酯共聚物的聚合研究 总被引:1,自引:0,他引:1
利用过氧化苯甲酰为引发剂探讨了甲基丙烯酸β-羟乙酯和丙烯酸长链烷基酯的自由基共聚合。重点讨论了合成条件如溶剂、沉淀剂、引发剂用量、单体配比、反应时间等对共聚反应的影响以及各种聚合条件对该共聚物的组成、结构和性能的影响。并用IR,GPC,^13CNMR等手段对共聚物进行了表征。 相似文献
63.
Jian Wang Xing‐You Xu Lu‐De Lu Xu‐Jie Yang Wei‐Xing Ma Xiang‐Ning Cui 《Surface and interface analysis : SIA》2007,39(6):482-486
The streaming potential of supersaturated solution of binary carboxylic acids, which have even carbon atoms, was determined to characterize crystallization under different temperatures. The value of the streaming potential was related to the type and solubility of the acids and the starting temperature of crystallization, and was easily influenced by the pressure difference of the liquid or the rate of temperature decline. When the temperature was declined to the point where a crystal nucleus appeared, the streaming potential reached the minimum. Thereafter, as the temperature was sequentially lowered, some minicrystals grew, and the streaming potential presented an ascendant tendency. The higher the starting temperature of the acids saturated solution, the higher is the temperature corresponding to the streaming potential minimum. The less the carbon atoms in the acids and the greater the solubility of the acids are, the higher is the temperature of the streaming potential minimum. Copyright © 2007 John Wiley & Sons, Ltd. 相似文献
64.
Zhixian Zhou Hongna Han Tiesheng Li Yanjun Xing Yangjie Wu Xian Xin Zhang Reed M. Izatt N. Kent Dalley Jerald S. Bradshaw Weijie Chai Cunheng He 《Structural chemistry》1999,10(3):177-185
Reactions of CsI and HgI2 with benzo-15-crown-5 (B15C5) and 15-crown-5 (15C5) in an ethanol-acetone mixture produced [Cs(B15C5)2]2[Hg2I6] (1) and {[Cs(15C5)]2[Hg2I6]}n (2), respectively. The structures of the two complexes are quite different. Molar ratios of Cs+ : crown ether are 1 : 2 in 1 and 1 : 1 in 2. Complex 1 consists of two Cs(B15C5)
2
+
cations and a Hg2I
6
2-
anion. Cs+ lies between the two crown-5 ligands, resulting in a sandwich-type cation. Cationic Cs(B15C5)
2
+
and anionic Hg2I
6
2-
are linked together by electrostatic interactions and the complex 1 is an ion pair compound. Complex 2 consists of infinite [Cs(15C5)]2[Hg2I6] units. Each structural unit contains two Cs(15C5)+ cations and a Hg2I
6
2-
anion. Cs+ is coordinated by five oxygen atoms of 15C5, three iodine atoms of Hg2I
6
2-
, and an iodine atom of Hg2I
6
2-
in an adjacent structural unit. The interactions between the Cs+ of Cs(15C5)+ and an I– in Hg2I
6
2-
from adjacent structural units polymerize the complex 2, resulting in a one-dimensional network structure. The anions of Hg2I
6
2-
in both complexes are similar. The two mercury atoms are linked through two bridging iodine atoms and each mercury is also coordinated by two terminal iodines. Crystal data for 1: space group P21/c (No. 14), a = 12.253(4), b = 20.945(7), c = 16.110(6) Å, = 111.0(1)°, V = 3860 Å3, Z = 4, R = 0.082 (R
w = 0.089). Crystal data for 2: space group P21/c (No. 14), a = 12.157(4), b = 8.546(4), c = 20.666(6) Å, = 91.54(3)°, V = 2146 Å3, Z = 4, R = 0.034 (R
w = 0.048). 相似文献
65.
Allyloxy bisbenzo 16-crown-5 trimethoxysilane was first used as precursor to prepare the sol-gel-derived bisbenzo crown ether/hydroxyl-terminated silicone oil (OH-TSO) SPME coating. The coating procedure involving sol solution composition and conditioning process was presented. Compared with commercial SPME stationary phases, the new coatings showed higher extraction efficiency and therefore could provide higher sensitivity for organphosphorous pesticides (OPs). Limits of detection (LODs) were in the range of 0.003-1.0 ng/g for these OPs in food samples (honey, juice, orange and pakchoi). The optimal extraction conditions of the new coatings to OPs in these samples were investigated by adjusting extraction time, salt addition, extraction temperature, and dilution ratios of samples with distilled water by using SPME coupled with gas chromatography (GC)-flame photometric detection (FPD). The method was applied to determine the concentrations of OPs in real samples. 相似文献
66.
67.
Sesquiterpene Lactone Glycosides from Carpesium macrocephalum 总被引:1,自引:0,他引:1
Two new sesquiterpene lactone glycosides were isolated from the seeds of Carpesium meacrocephalum. Their structures were elucidated as 2α-O-β-D-glucopyranosy-5α,11αH-eudesma-4(15)-en-12,8β-olide and 2α-O-β-D-glucopyranosy-5αH-eudesma-4(15),11(13)-dien-12,8β-olide by spectral methods (HRMS,1D and 2D NMR). 相似文献
68.
Xing Yong Wang Jing Nan Cui Wei Min Ren Feng Li Chun Liang Lu Xu Hong Qian State Key Laboratory of Fine Chemicals Dalian University of Technology Dalian China School of Chemical Engineering Technology China University of Mining & Technology Xuzhou China Shanghai Key Laboratory of Chemical Biology East China University of Science Technology Shanghai China 《中国化学快报》2007,18(6):681-684
Baker's yeast mediated reduction of acenaphthenequinone within 4-10 h afforded mono-hydroxyacenaphthenone mainly with low enantioselectivity, the substrate and mono-hydroxyacenaphthenone product almost converted to dihydroxyacenaphthene after 48 h. By control of the reaction time and in the presence of DMF as co-solvent, the reduction of 6-substituted acenaphthenequinones under vigorous agitation afforded the corresponding 2-hydroxyacenaphthenones in 24-84% yields with 10-93% ee. 相似文献
69.
Intracellular delivery of enzymes is essential for protein-based diagnostic and therapeutic applications. Protein-spherical nucleic acids (ProSNAs) defined by protein core and dense shell of oligonucleotides have been demonstrated as a promising vehicle-free enzyme delivery platform. In this work, we reported a crosslinking strategy to vastly improve both delivery efficiency and intracellular sensor performance of ProSNA. By assembling individual ProSNA with lactate oxidase (LOX) core into a nanoscale particle, termed as crosslinked SNA (X-SNA), the enzyme delivery efficiency increased up to 5–6 times higher. The LOX X-SNA was later demonstrated as a ratiometric probe for quantitative detection of lactate in living cells. More importantly, X-SNA probe showed significantly improved sensor performance with signal-to-noise ratio 4 times as high as ProSNA when detecting intracellular lactate.By crosslinking protein spherical nucleic acid (SNA) into a supramolecular architecture X-SNA, the intracellular enzyme delivery efficiency was significantly enhanced, showing 3–4 times higher signal-to-noise ratio in detecting intracellular lactate. 相似文献
70.
Capillary electrophoresis with end-column amperometric detection of urinary 8-hydroxy-2'-deoxyguanosine 总被引:1,自引:0,他引:1
Urinary 8-hydroxy-2'-deoxyguanosine (8OHdG) is an excellent marker of oxidative DNA damage. Until now, urinary 8OHdG has been measured by high-performance liquid chromatography with electrochemical detection. A simple and sensitive method for the analysis of urinary 8OHdG by capillary electrophoresis with end-column amperometric detection has been developed in our laboratory. A single-step solid-phase extraction procedure was optimized and used for extracting 8OHdG from human urine. To improve the sensitivity of this method, a new focusing technique based on a dynamic pH junction was used. The limit of detection was 20 nM (signal-to-noise ratio S/N = 3), the linear range was 50 nM-10 microM, and the correlation coefficient was better than 0.999. The relative standard deviation (RSD) was found to be 0.57% for migration time, and 4.79% for peak current. To show the usefulness of the method, the urinary concentration of 8OHdG in nine healthy persons and ten cancer patients was determined. The urinary concentration of 8OHdG in cancer patients was significantly higher than that in healthy persons. 相似文献