共查询到19条相似文献,搜索用时 62 毫秒
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脱羧氯雷他定 (DCL)是一种有效的非镇定性抗组织胺 ,对过敏性鼻炎 ,糖尿病、咳嗽、普通感冒、流行性感冒、关节痛及其它不适症状都有很好的疗效[1~2 ] 。它克服了氯雷他定、酮康唑、红霉素、伊曲康唑等易引发黑色素瘤、纤维肉瘤、胃刺激、肥胖症、心律失调、传导紊乱等症状的缺点。且它的使用剂量只有氯雷他定的十分之一 ,有很好的市场前景和实际应用价值。MarkW .Holladayetal[3] 在水溶液中由酸、碱催化得到了脱羧氯雷他定 ,但无具体操作和反应结果报道。A .K .GunnarAberg[1] 直接用KOH在绝对无水… 相似文献
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以地氯雷他定和对硝基苯甲酰氯为原料,三乙胺为缚酸剂,经N-酰化反应制得{4-[8-氯-5H-苯并[5,6]环庚并[1,2-b]吡啶-11(6H)-亚基]哌啶-1-基}(4-硝基苯基)甲酮(3);3在酸性条件下经SnCl2还原得中间体(4)。以吡啶为缚酸剂和溶剂,4与烷基酰氯(或苯酰氯)经酰化反应合成了7个具有潜在AVP-V2受体拮抗活性的新型地氯雷他定酰胺衍生物(6a~6g),其结构经1H NMR和HR-MS表征。SD大鼠利尿活性实验表明,6a~6g均有一定的利尿活性,其中N-【4-{4-[8-氯-5H-苯并[5,6]环庚烷并[1,2-b]吡啶-11(6H)-亚基]哌啶-1-羰基}苯基】丙酰胺的利尿活性与托伐普坦相当。 相似文献
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顶空毛细管气相色谱法测定氯雷他定中9种有机溶剂的残留量 总被引:1,自引:0,他引:1
提出了顶空毛细管气相色谱法测定氯雷他定中乙醚、异丙醇、乙腈、叔丁醇、乙酸乙酯、四氢呋喃、环己烷、三乙胺和甲苯的残留量.采用DB-624毛细管柱(30 mX0.53 inIil,3μm),程序升温,以N、N二甲基甲酰胺(DMF)为溶剂,9种溶剂的平均回收率分别为98.2%,98.8%,106.0%,99.0%,97.7%,95.4%,95.1%,93.O%,100.6%,检出限分别为0.056,0.67,0.61,0.45,0.33,0.16,0.041,0.28,0.20 mg·L-1,测定限分别为0.17,2.0,1.9,1.1,1.1,0.54,0.13,0.90,0.69 mg·L-1. 相似文献
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气相色谱法测定脱羧氯雷他定中有机溶剂残留量 总被引:5,自引:0,他引:5
采用气相色谱技术建立脱酸氯雷他定中5种有机溶剂乙醇、乙腈、乙酸乙酯、四氢呋喃、甲苯残留量的测定方法;以N,N-二甲基甲酰胺为溶剂,苯为内标,在聚乙二醇-20M柱和OV-101毛细管柱串联柱上,程序升温可有效分离各组分,氢火焰检测器检测;各有机溶剂在5-200mg/L范围内线性良好(r=0.999),在高、中、低3个浓度水平上的平均回收率分别为乙醇98.6%、乙腈98.9%、乙酸乙酯105%、四氢呋喃98.4%、甲苯100%;检出限分别为25、50、25、25、10μg/g。 相似文献
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8-氯-5,6-二氢-11H-苯并[5,6]环庚烷并[1,2-b]吡啶-11-酮是合成氯雷他定、地氯雷他定、卢帕他定等第二代抗组胺药的重要中间体。本文对其合成方法进行了综述。 相似文献
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以5步反应从邻碘苯甲酸乙酯合成了9,10-二氢-9,9,10,10-双(γ-丁内酯)菲,减少了3步反应,总产率提高7%.又由邻碘苯甲酰氯与乙烷-1,1,2-三羧酸三乙酯缩合,继以消除两个乙酯基合成Dallacker双内酯,反应减少一步,产率则增高13%.还研究了联苯-2,2-二甲酰氯分别与乙烷-1,1,2-三羧酸三乙酯和氰基琥珀酸二乙酯的缩合,均能得到良好的产率. 相似文献
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Surajit Some 《Tetrahedron letters》2006,47(7):1221-1224
A convenient synthetic approach to substituted benzene derivatives by modified Ullmann cross-coupling of 2-bromobenzaldehyde and bromovinylaldehydes followed by intramolecular McMurry coupling has been developed. 相似文献
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Hossein Reza Darabi Ali Reza Mohebbi Mohammad Bolourtchian 《Supramolecular chemistry》2013,25(6):465-468
The synthesis, properties and energy-optimized structure of stilbenophanes 1a–3a are reported. 1H NMR spectroscopy of 1a shows it contains vinylic protons (unlike larger stilbenophanes), which appear as two doublets showing its unexpected configuration. Protons of the methylene bridge of 1b are also observed at different chemical shift, showing that they are diastereomeric protons. It is also found that the stereochemical outcome of the intramolecular McMurry reaction is strongly influenced by the length of the alkyl bridge. 相似文献
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Thamina Akther Md.Monarul Islam Taisuke Matsumoto Junji Tanaka Pierre Thuéry Carl Redshaw Takehiko Yamato 《Tetrahedron》2018,74(2):329-335
The reductive coupling reaction of 1,4-bis(3-acetyl-5-tert-butyl-2-methoxyphenyl)butane 3 was carried out using TiCl4-Zn in pyridine followed by a McMurry coupling reaction to afford the compounds anti and syn 1,2-dimethyl[2.4]MCP-1-ene 4. Bromination of 4 with BTMA-Br3 in dry CH2Cl2 afforded the interesting compound 1,2-bis-(bromomethyl)-5,15-di-tert-butyl-8,18-dimethoxy[2.4]MCP-1-ene 6 and consecutive debromination with Zn and AcOH in CH2Cl2 solution afforded the stable solid 5,15-di-tert-butyl-8,18-dimethoxy-1,2-dimethylene[2.4]MCP 7 in 89% yield. Compound 7 was conveniently employed in a Diels–Alder reaction with dimethyl acetylenedicarboxylate (DMAD) to provide 2-(3′,6′-dihydrobenzo)-5,15-di-tert-butyl-8,18-dimethoxy[2.4]MCP-4′,5′-dimethylcarboxylate 8 in good yield. Diels–Alder adduct 8 was converted into a novel and inherently chiral areno-bridged compound [2.4]MCP 9 by aromatization. The chirality of the two conformers was characterized by circular dichroism (CD) spectra of the separated enantiomer which are perfect mirror images of each other. 相似文献
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L. I. Belen'kii G. P. Gromova A. V. Kolotaev B. V. Nabatov M. M. Krayushkin 《Russian Chemical Bulletin》2005,54(5):1208-1213
Tetrakis(3,5-dimethyl-2-thienyl)ethylene and tetrakis(2,5-dimethyl-3-thienyl)ethylene were obtained from the corresponding
dithienyl ketones by the McMurry reaction. The photochromic properties of the compounds obtained were studied.
Dedicated to the Academician N. K. Kochetkov on the occasion of his 90th birthday.
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Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 5, pp. 1177–1181, May, 2005. 相似文献
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(−)-β-Caryophyllene has been converted into three stereoisomers of a new bicyclic compound that is structurally related to the known macrocyclic diterpene, flexibilene, in the same way β-caryophyllene is related to humulene. Key steps are selective cleavage of caryophyllene, addition of a five carbon component by a Wittig reaction and McMurry cyclization. 相似文献
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L. Omar M. I. El-Barghouthi N. A. Masoud A. A. Abdoh M. M. Al Omari M. B. Zughul A. A. Badwan 《Journal of solution chemistry》2007,36(5):605-616
The extent and mode of solubility enhancement exerted by the cyclodextrins (α-, β-, γ-, and HP-β-CDs) on loratadine (Lort) have been experimentally measured under controlled conditions in buffered aqueous solutions. Rigorous
nonlinear regression analysis of the phase solubility diagrams obtained in 0.1 mol⋅L−1 phosphate buffer at pH=7.0 and 25 °C revealed the following: neutral Lort (pK
a
=4.6) tends to form soluble 1:1 and 1:2 Lort/CD complexes with all four of the examined CDs, where complex stability follows
the decreasing order β-CD>HP-β-CD>γ-CD>α-CD. The hydrophobic character of Lort constitutes about 66% of the driving force for complex formation whereas specific interactions
contribute 11.2 kJ⋅mol−1 towards the stability of the complexes. Thermodynamic studies showed that Lort/CD complex formation was favored by large
enthalpic contributions but was impeded by negative entropic changes. Dissolution studies indicate that the dissolution rate
of Lort from the freeze-dried Lort/β-CD complex is significantly higher than that of the corresponding physical mixture. Both DSC studies and molecular mechanical
modeling of Lort/β-CD interactions were carried out to explore the possible formation of inclusion complexes. 相似文献
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A new polyoxygenated crownophane has been synthesized from syringaldehyde and diethyleneglycol by means of McMurry pinacol reaction, whereas ring closing metathesis with Grubbs’ catalyst failed in producing the macrocyclization to the corresponding stilbenophane. The NMR data of the crownophane show a restricted conformational space accessible to the phenyl rings. 相似文献