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971.
972.
Yan B Collins N Wheatley J Irving M Leopold K Chan C Shornikov A Fang L Lee A Stock M Zhao J 《Journal of combinatorial chemistry》2004,6(2):255-261
We have developed a high-throughput purification system to purify combinatorial libraries at a 50-100-mg scale with a throughput of 250 samples/instrument/day. We applied an accelerated retention window method to shorten the purification time and targeted one fraction per injection to simplify data tracking, lower QC workload, and simplify the postpurification processing. First, we determined the accurate retention time and peak height for all compounds using an eight-channel parallel LC/UV/MS system, and calculated the specific preparative HPLC conditions for individual compounds. The preparative HPLC conditions include the compound-specific gradient segment for individual compounds with a fixed gradient slope and the compound-specific UV or ELSD threshold for triggering a fraction collection device. A unique solvent composition or solvent strength was programmed for each compound in the preparative HPLC in order to elute all compounds at the same target time. Considering the possible deviation of the predicted retention time, a 1-min window around the target time was set to collect peaks above a threshold based on UV or ELSD detection. Dual column preparative instruments were used to maximize throughput. We have purified more than 500 000 druglike compounds using this system in the past 3 years. We report various components of this high-throughput purification system and some of our purification results. 相似文献
973.
丙烯在ZSM-5沸石上齐聚反应的研究 Ⅰ. 模板剂用量对丙烯齐聚反应的影响 总被引:3,自引:2,他引:3
考察了不同正丁胺(NBA)模板剂用量合成ZSM-5沸石的物化特性和催化性能。采用XRD、SEM、NH3-TPD和BET等手段对合成样品的物化特性进行了表征。结果表明,模板剂与SiO2摩尔比在0.67~0.22时合成的ZSM-5沸石结晶度高于90%;随着模板剂用量的减少,ZSM-5沸石的平均粒径减小,强酸量也存在相同的趋势。丙烯齐聚反应评价结果显示,模板剂用量对合成ZSM-5沸石的催化活性有显著影响,模板剂与SiO2摩尔比在0.67~0.45之间合成的沸石催化性能较好。 相似文献
974.
WU Yan-Qi LOU Ning LI Yu 《有机化学》2003,23(Z1):442-442
From the ethanolic extract of the whole plant of Anaphalis aureo-punctata, a new acylated flavonoid glycoside 3-O-kaempferol-3-O-acetyl-6-O-(p-coumaroyl)-β-D-glucopyranoside (1), and five known phenolic compounds 3-O-kaempferol-6- O- ( p-coumaroyl )-β-D-glucopyranoside ( 2 ), kaempferol-3- O-β-D-glucopyranoside 3,6-(4′-hydroxystyryl)-4-methoxy-2-pyrone (4), 2H-pyran-2-one, 6-[ 2-( 4-(β-D-glucopyranosyloxy ) phenyl ) ethenyl ]-4-methoxy-( E ) (5) and 4-hydroxy-3-methoxycinnamic hexacosyl ester (6) were isolated. Their structures were established by spectral methods (UV, IR, MS, 1D, 2D-NMR). The flavonoid glycosides, 1, 2 and 3 showed markedly inhibited oxidative DNA strand breaks induced by Fenton reaction and NADH/PMS in a concentration-dependent manner. 相似文献
975.
Polyvinyl alcohol carriers bearing active amide and active ester groups were prepared by acetaliza-tion of granular macro-reticular water-insolub1e PVA with glyoxylic acid or p-formylbenzoic acidand further activation reaction with benzotriazole or N-hydroxysuccinimide using DCCI as con-densation agent. The active amides or active esters obtained were easy to react with amines suchas n-butylamine or proteins under mild condition. Ovomucoid, an inhibitor of trypsin was immo-bilized on the above-obtained reactive PVA carrier to give effective affinity adsorbent for the separa-tion or purification of trypsin. 相似文献
976.
CdSe纳米线阵列的制备及其表征(英) 总被引:1,自引:0,他引:1
通过在含有SeSO32-和Cd2+的室温水溶液中,用模板-电沉积法在纳米孔阵列阳极氧化铝膜(AAM)模板中制备了高有序性的CdSe纳米线阵列,并对其形貌、结构和组分进行了表征。扫描电子显微镜(SEM)和透射电子显微镜(TEM)结果表明,纳米线阵列中的CdSe纳米线具有相同的长度和直径,分别对应于使用的AAM模板的厚度和孔径;X-射线衍射(XRD)和X-射线能谱(EDAX)结果表明,CdSe纳米线中Cd和Se的化学组成非常接近于1∶1,其结构为立方CdSe。另外,对模板-电沉积法制备CdSe纳米线的机理进行了讨论。 相似文献
977.
A New Asterosaponin from the Starfish Culcita novaeguineae 总被引:1,自引:0,他引:1
HaiFengTANG YangHuaYI LingLI PengSUN DaZhengZHOU BaoShuLIU 《中国化学快报》2005,16(5):619-622
A new asterosaponin named novaeguinoside A, along with a known saponin, asteronyl pentaglycoside sulfate, was isolated from the starfish Culcita novaeguineae. The new compound was identitied to be sodium 6α-O-{β-D-fucopyranosyl-(1→2)-β-D-fucopyranosyl-(1→4)-[β-D-quinovopyranosyl-(1→2)]-β-D-xylopyranosyl-(1→3)-[β-D-quinovopyranosyl}-5α-pregn-9(11)-en-20-one-3β-yl-sulfate by extensive spectral analysis and chemical evidence. 相似文献
978.
Several novel N′-[(1-ferrocenylethylidene)amino]-N′-β-D-glycopyranosylthioureas have been efficiently synthesized via a six-step procedure, utilizing three monosaccharides (D-glucose, D-galactose and D-xylose) as starting materials, respectively. They have been preliminarily determined to display biological activity against certain fungi. The target compounds have been unambiguously characterized by spectroscopic method and elemental analysis. An initially alternative synthetic route, which was seemingly reasonable, has been excluded due to its inefficiency. 相似文献
979.
哌嗪取代卟啉的合成、表征及其抗癌活性 总被引:2,自引:0,他引:2
设计并合成了6个具有抗癌活性的哌嗪取代卟啉化合物,分别为5,10,15,20-四[4-(4'-乙基哌嗪基)苯基]卟啉(TEPPH2,8a),5,10,15,20-四[4-(4'-丁基哌嗪基)苯基]卟啉(TBPPH2,8b),5,10,15,20-四[4-(4'-庚基哌嗪基)苯基]卟啉(THPPH2,8c),5,10,15,20-四[4-(4'-苯基哌嗪基)苯基]卟啉(TPhPPH2,8d),5-[4-(4'-乙基哌嗪基)苯基]-10,15,20-三苯基卟啉(EPTPPH2,8e)和5-[4-(4'-丁基哌嗪基)苯基]-10,15,20-三苯基卟啉(BPTPPH2,8f).这些卟啉化合物都由取代苯甲醛与吡咯缩合而成,每一个卟啉分子中含有一个或四个具有抗癌活性的取代哌嗪结构,结构经元素分析,MS,1H NMR,IR和UV-vis等表征.初步的生物活性研究表明,这些化合物具有一定的抗癌活性,因而在医学上可能具有潜在应用前景. 相似文献
980.