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目的 研究N~6-苯甲酰基-2′-叔丁基二甲基硅氧基腺苷-3′-H-膦酸的合成工艺。方法 以腺苷为起始原料,先对腺苷的嘌呤氨基进行苯甲酰基保护,再分别向腺苷的5′位和2′位引入二甲氧基三苯甲基(DMT)和叔丁基二甲基硅基(TBDMS)保护基,制备得到关键中间体N~6-苯甲酰基-5′-二甲氧基三苯甲氧基-2′-叔丁基二甲基硅氧基腺苷(3)。中间体3与磷试剂2-氯-4H-1,3,2-苯并二氧磷杂环己烷-4-酮反应引入膦酸基团,最后使用二氯乙酸脱除DMT保护基得到目标产物。结果 经过5步反应得到了目标化合物N~6-苯甲酰基-2′-叔丁基二甲基硅氧基腺苷-3′-H-膦酸,并利用~1H-NMR、~(31)P-NMR、质谱等方法确证了其结构。本合成工艺的总收率为35.7%,目标化合物的质量分数为98.5%。结论 该合成工艺与原有方法相比步骤短,操作简单,具有良好的应用前景。 相似文献
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邻羟基苯甲酰胺和环己酮经酰化、与(3R,4R)-4-乙酰氧基-3-[(1R)-1-(叔丁基二甲硅氧基)乙基]氮杂环丁烷-2-酮(4)缩合、水解得(3S,4S)-4-[(1R)-1-羧乙基]-3-[(1R)-1-(叔丁基二甲硅氧基)乙基]氮杂环丁烷-2-酮(6).6再经缩合、脱保护、环合、烯醇化及酯化得1β-甲基碳青霉烯双环母核,总收率约29%(以邻羟基苯甲酰胺计). 相似文献
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3-甲基△~2环已烯-1-酮(4)与1,4-二溴丁烷在氨钠,液氨中或在叔丁醇钾的苯溶液中进行螺环化反应,得到螺环化合物5a 5b以及双螺环化合物6a 6b。经定量催化氢化;羰基与三甲基硅氰加成反应;硅醚水解;脱水和腈基水解,合成了10-甲基-螺[4.5]-癸-6-烯-6-羧酸(11)。药理试验表明该化合物有一定的麻醉催眠作用。 相似文献
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3-甲基△2环已烯-1-酮(4)与1,4-二溴丁烷在氨钠,液氨中或在叔丁醇钾的苯溶液中进行螺环化反应,得到螺环化合物5a+5b以及双螺环化合物6a+6b。经定量催化氢化;羰基与三甲基硅氰加成反应;硅醚水解;脱水和腈基水解,合成了10-甲基-螺[4.5]-癸-6-烯-6-羧酸(11)。药理试验表明该化合物有一定的麻醉催眠作用。 相似文献
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本文报道用三价磷试剂与保护的鸟嘌呤核苷反应,经碘氧化生成鸟嘌呤核苷-3′,5′-环磷酸酯和磷酰胺,并对它们的生物活性做了初步研究,N~2-二甲胺基甲烯基-2′-叔丁基二甲基硅基鸟嘌呤核苷-3′,5′-环磷酸酯和磷酰胺对小鼠肝癌腹水细胞的DNA和RNA合成有一定的抑制作用。N~2-二甲胺基甲烯基鸟嘌呤核苷-3′,5′’-环磷酸丁酯的两个磷原子构型不同的异构体可激活腺苷酸环化酶,使大鼠成骨肉瘸细胞株ROS 17/2.8的cAMP水平增高。 相似文献
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《Expert opinion on therapeutic patents》2013,23(1):113-117
Crystalline forms A and D of N-[2-[[(2,3-difluoropheny)methyl]thio]-6-{[(1R,2S)-2,3-dihydroxy-1-methylpropyl]oxy}-4-pyrimidinyl]-1-azetidinesulfonamide are claimed. The compound is a previously disclosed CXCR2 chemokine receptor antagonist and is claimed to be useful in the treatment of inflammatory diseases such as chronic obstructive pulmonary disease (COPD). 相似文献
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目的 研究海绵Agelas sp.的化学成分。方法 运用乙醇提取、硅胶、Sephadex-LH20色谱柱、HPLC等多种方法进行分离和纯化,根据理化性质和波谱数据进行结构鉴定。结果 分离得到9个化合物,经结构鉴定分别为4,5-二溴吡咯-2-甲酰胺(1)、4,5-二溴吡咯-2-甲酸(2)、4,5-二溴吡咯-2-甲酸甲酯(3)、N-(4,5-二溴-2-吡咯甲酰基)甘氨酸甲酯(4)、1-(4,5-二溴-2-吡咯甲酰胺基)丙酸甲酯(5)、1-(4,5-二溴-2-吡咯甲酰胺基)丙酸乙酯(6)、异吲哚-1,3-二酮(7)、2(3H)-苯并噻唑酮(8)和manzacidin C(9)。结论 化合物4~9为首次从该属海绵中分离得到,其中化合物4~6为新天然产物。 相似文献
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为了保证克拉维酸钾(1)的质量,本研究合成了欧洲药典收载的有关物质F,即4-[[[4-(2-羟乙基)-1H-吡咯-3-羰基]-氧]甲基]-1H-吡咯-3-羧酸。4-氯乙酰乙酸甲酯(2)与原甲酸三乙酯反应得4-氯-2-(二乙氧基甲基)-3-氧代丁酸甲酯(3),3与甘氨酸反应得烯胺。烯胺在乙酸酐中回流,经环合、脱羧得4-(氯甲基)-1H-吡咯-3-羧酸甲酯(5)。5和1的降解产物4-(2-羟乙基)-1H-吡咯-3-羧酸(8)反应得[4-(甲氧基羰基)-1H-吡咯-3-基]甲基4-(2-羟乙基)-1H-吡咯-3-羧酸甲酯(6),6经水解得有关物质F。产物结构经MS、1H NMR和13C NMR确证。 相似文献
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Malhotra M Sharma R Sanduja M Hans P Sharma S Deep A 《Acta poloniae pharmaceutica》2012,69(2):363-368
Seventeen analogues of benzylidene were synthesized and evaluated for in vitro hydrogen peroxide scavenging activity. The structure of the newly synthesized compounds were confirmed by elemental and spectral (IR, 1H-NMR, 13C-NMR) studies. The antioxidant activity of the titled compounds was evaluated. Compounds: 4h--N'-[2-amino-3-(morpholinomethyl)benzylidene]isonicotinohydrazide, 4p 7-(4-(2-amino-3-[(2-isonicotinoylhydrazono)methyl]benzyl}piperazin-1-yl)-1-cyclopropyl-6-fluoro-4-oxo-1,4-dihydroquino- line-3-carboxylic acid and 4q 7-(4-{2-amino-3-[(2 isonicotinoylhydrazono)methyl]benzyl} piperazin-1-yl)-1-ethyl-6,8-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid were the most active compounds with significant hydrogen peroxide scavenging activity. 相似文献
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Naheed Riaz Shehla Parveen Muhammad Saleem Muhammad Shaiq Ali Abdul Malik Muhammad Ashraf 《Journal of Asian natural products research》2013,15(6):545-554
Four new sphingolipids: nudicaulin A [(2S,3S,4R,14E)-2-{[octadecanoyl]amino}tetraeicos-14-ene-1,3,4-triol; 1], nudicaulin B [(2S,3S,4R,14E)-2-{[(2R)-2-hydroxyoctadecanoyl]amino}tetraeicos-14-ene-1,3,4-triol; 2], nudicaulin C [(2S,3S,4R,14E)-2-{[(2R)-2-hydroxyoctadecanoyl]amino}tetraeicos-14-ene-1,3,4-triol-1-O-β-d-glucopyranoside; 3], and nudicaulin D [(2S,3S,4R)-2-{[(2R,3S,12E)-2,3-dihydroxyeicos-12-enoyl]amino}octadecane-1,3,4-triol; 4] together with 1-hexatriacontanol, β-sitosterol, octadecyl 4-hydroxycinnamate, elaidic acid, cholesta-5,22-diene-3,7-diol, oleanolic acid, apigenin, and β-sitosterol 3-O-β-d-glucopyranoside were isolated from the methanolic extract of the whole plant of Launaea nudicaulis. Their structures were elucidated using 1H and 13C NMR spectra and 2D NMR analyses (HMQC, HMBC, and COSY) in combination with mass spectrometry (EI-MS, HR-EI-MS, FAB-MS, and HR-FAB-MS) experiments and comparison with literature data of related compounds. Compounds 1–4 displayed moderate inhibitory potential against enzyme lipoxygenase in concentration-dependent manner with IC50 value ranges 103–193 μM. 相似文献
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Julian Schwarzkopf Tom Sundermann Martina Arnsmann Walburga Hanekamp Jörg Fabian Jan Heidemann Anna Friederike Pott Dominik Bettenworth Matthias Lehr 《Medicinal chemistry research》2014,23(12):5250-5262
Cytosolic phospholipase A2α is a serine hydrolase involved in the generation of pro-inflammatory lipid mediators. Here, we describe structure–activity relationship studies on a series of carbamate-substituted indazole-5-carboxylic acid inhibitors of this enzyme. Bioavailability experiments in mice with 1-(3-(4-butylphenoxy)-2-{[(ethylthio)carbonyl]amino}propyl)indazole-5-carboxylic acid (14) revealed a high rate of glucuronidation and biliary excretion of this compound. Replacement of the rigid aromatic carboxylic acid system by a more flexible aliphatic one led to substances with a significantly increased in vitro stability against metabolic glucuronidation. 相似文献
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目的 合成抗高血压药坎地沙坦的前药坎地沙坦酯。方法 以三苯甲基坎地沙坦为起始原料, 经酯化、脱保护基得到1-氯乙基-2-乙氧基-3-[(2’-(1H-四氮唑-5-基)联苯基-4-基)甲基]-3H-苯并咪唑-4-酯,该中间体与环己基碳酸单酯反应得到candesartan cilexitil。结果与结论 总收率为42.1%,目标化合物的结构经核磁共振氢谱,质谱确证。 相似文献
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The title compounds 2-substituted phenyl-3-{1-cyclopropyl-6-fluoro-7-[4-(4-methoxyphenylpiperazin-1-yl]-4-oxo-1,4-dihydroquinoline}
carboxamido-1,3-thiazolidin-4-ones 6a–j have been synthesized from lead molecule 7-chloro-1-cyclopropyl-6-fluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid 1; this reacted with thionyl chloride to give acid chloride 2 and with hydrazine hydrate to afford hydrazide 3. The hydrazide 3 on condensation with substituted aromatic aldehydes a–j gave Schiff base; these on reaction with N-(4-methoxyphenyl) piperazine and thioglycolic acid furnished title compounds 6a–j. All of the synthesized compounds have been established by elemental analysis. IR and NMR spectral data and have been screened
for antifungal and antibacterial activities. 相似文献