共查询到20条相似文献,搜索用时 156 毫秒
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1-(5-萘酚-7-磺酸)-3-[4-(苯基偶氮)苯基]-三氮烯的合成及与阳离子表面活性剂的显色反应 总被引:31,自引:0,他引:31
报道了1-(5-萘酚-7-磺酸)-3-[4-(苯基偶氮)苯基]-三氮烯(NASAPAPT)的合成,研究了该试剂与阳离子表面活性剂溴化十二烷基二甲基苄铵(DDMBAB),溴化十六烷基三甲铵(CTMAB)、溴化十六烷基吡啶(CPB)、溴化十四烷基吡啶(TPB)显色反应的条件。测定了显色反应的灵敏度,符合比尔定律的范围。建立了光度法测定微量阳离子表面活性剂的新方法。 相似文献
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6-甲基-[1,3]二氧戊环并[4,5-g]喹啉-7-甲酸乙酯(1)与N-溴代丁二酰亚胺(NBS)在150W白炽灯照射的条件下有效的发生自由基溴化反应,以较好的收率(75%)得到想要的单溴化产品6-(溴甲基)-[1,3]二氧戊环并[4,5-g]喹啉-7-甲酸乙酯(2)。本文所开发的自由基溴化方法与文献相比,单溴化产品的收率提高了46%。另外,该溴化反应中所生成的少量副产品也进行了分离提纯,其结构经波谱分析证实为9-溴-6-甲基-[1,3]二氧戊环并[4,5-g]喹啉-7-甲酸乙酯(3)。 相似文献
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Maël Penhoat 《Tetrahedron letters》2005,46(48):8385-8389
New and mild conditions to prepare chiral bicyclic lactams in high yields and high diastereoselectivities are reported herein. This approach based on the activation of the carboxylic acid by means of Mukaiyama’s reagent is an excellent alternative to Meyers’ dehydrating conditions and provide the main advantage to work at lower temperature (40 °C). Higher diastereoselectivity was obtained with 5,7-bicyclic lactams (de = 82% instead of 44% under standard dehydrating conditions). 相似文献
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以布洛芬(IPF)和扑热息痛(PCM)为原料,无水丙酮和乙酸乙酯为溶剂,二环己基碳二亚胺(DCC)为脱水剂,4-二甲氨基吡啶(DMAP)为催化剂,合成了布洛芬-扑热息痛孪药(PHI),以重结晶法对目标产物进行纯化,产物结构经IR和1H NMR确定。 探讨了原料比例、脱水剂用量、催化剂用量、反应时间和溶媒用量对目标物产率的影响,并采用正交试验筛选最优合成工艺,最终确定的最优反应条件为:n(PCM)∶n(IPF)=1∶1.5,催化剂的最佳用量为布洛芬质量的10%,反应时间为8 h,溶媒体积为70 mL(V(乙酸乙酯)∶V(丙酮)=1∶1),在该条件下,目标物PHI的产率为66.53%。 相似文献
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BinFU DaMingDU QingXIA 《中国化学快报》2004,15(4):383-385
The synthesis of bis(oxazoline) dicarboxylate derivatives was investigated.Diethyl-aminosulfur trifluoride (DAST) was used as a convenient cyclization reagent in the synthesis of bis(oxazoline) dicarboxylate derivatives,which can not be obtained by the general method using MsC1 and Et3N as dehydrating cyclization reagent. 相似文献
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《Mendeleev Communications》2022,32(1):54-56
The combination of a dibutyltin(IV) oxide catalyst with an ortho ester as the dehydrating agent exhibited high activity for the direct synthesis of diethyl carbonate from CO2 and ethanol in 78% yield. With water as a by-product limiting the reaction, a recoverable dehydrating agent is required. When alkoxysilanes were employed for this purpose, various dialkyl carbonates were obtained in yields of 33–45%. 相似文献
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Synthesis of N-tosylimines of arylaldehydes was carried out by the reaction of arylaldehydes and p-toluenesulfonamide in methylene chloride in the presence of trifluoroacetic anhydride as a dehydrating agent. 相似文献
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A new type of polymeric dehydrating reagent, readily prepared by the treatment of polymer-supported triphenylphosphine oxide with triflic anhydride, was found to be effective in a variety of dehydration reactions such as ester and amide formation; the polymer-supported triphenylphosphine oxide was easily recovered and reused several times without the loss of activity. 相似文献
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Dr. Klára Bednářová Dr. Iva Kejnovská Prof. Michaela Vorlíčková Dr. Daniel Renčiuk 《Chemistry (Weinheim an der Bergstrasse, Germany)》2019,25(58):13422-13428
Guanine quadruplexes, recently reported to form in vivo, represent a broad spectrum of non-canonical conformations of nucleic acids. The actual conformation might differ between water solutions and crowding or dehydrating solutions that better reflect the conditions in the cell. Here we show, using spectroscopic techniques, that most guanine substitutions prevent the conformational switch from antiparallel or hybrid forms to parallel ones when induced by dehydrating agents. The inhibitory effect does not depend on the position of the substitution, but, interestingly, on the type of substitution and, to some extent, on its destabilising potential. A parallel form might be induced in some cases by ligands such as N-methyl mesoporphyrin IX and even this ligand-induced switch is inhibited by guanine substitution. The ability or inability to have a conformation switch, based on actual conditions, might significantly influence potential conformation-dependent quadruplex interactions. 相似文献
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酚在碱性条件下与卤代烃反应生成相应的芳香醚,是典型的亲核取代反应,对于2,4-二硝基酚和二氟溴甲基膦酸二乙酯在碱性条件下的反应,其实验过程包括室温中和,甲苯回流脱水和亲核取代等三步反应。对产物进行了提纯和一系列的表征,结果发现主要生成了一种酚醚化合物。 相似文献
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Shikii K Seki H Yamaguchi K Disadee W Watanabe T Ishikawa T 《Chemical & pharmaceutical bulletin》2004,52(7):864-865
Polymer-supported (PS) reagents can be easily characterized using a cross polarization magic angle spinning method in solid state (13)C-NMR. The technique was applied to the characterization of PS-dimethylimidazolidinone, analogue to potential heterogeneous dehydrating agent. 相似文献
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Seung Tae Hong Hyung Sang Park Jong Sung Lim Youn-Woo Lee Masakazu Anpo Jae-Duck Kim 《Research on Chemical Intermediates》2006,32(8):737-747
The synthesis of dimethyl carbonate (DMC) from methanol and supercritical carbon dioxide over various base catalysts has been
studied. Compounds of group-I elements (Li, Na and K) were used as base catalysts. The promoter and the dehydrating agent
were also used to enhance the yield of DMC. The effects of the catalysts, promoter and dehydrating agent on the yield of DMC
were investigated. By-products such as dimethyl ether (DME) and C1–C2 hydrocarbons were formed with the DMC as a main product. The yield of DMC with different alkali metal catalysts ranked in
the following order: K > Na > Li. The catalysts of the metal-CO3 compounds were more effective than the metal-OH compounds in DMC synthesis. The maximum DMC yield reached up to about 12
mol% in the presence of K2CO3 (catalyst), CH3I (promoter) and 2,2-dimethoxypropane (dehydrating agent) at 130–140°C and 200 bar. The reaction mechanism of DMC synthesis
from methanol and supercritical carbon dioxide was proposed. 相似文献