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1.
以廉价易得的苦参碱为起始原料,经过开环、酯化反应、水解等步骤,得到4-((3aS,3aS,10aR)-2-(叔丁氧基羰基)十氢-(1H,4H)-吡啶并[1,6]萘啶-1-基)丁酸(5)。5再经过Curtius重排反应,得到叔丁基(1R,3aS,3aS,10aR)-1-(3-(((苄氧基)羰基)氨基)丙基)八氢-(1H,4H)-吡啶并[1,6]萘啶-2(3H)-羧酸叔丁酯(6)。然后,6脱去Cbz基团得到(1R,3aS,3aS,10aR)-1-(3-氨基丙基)八氢-(1H,4H)-吡啶并[1,6]二氮杂萘-2(3H)-羧酸叔丁酯(7),最后,7脱去Boc基团成功得到苦参碱衍生物的重要中间体3-((1R,3aS,3aS,10aR)-十氢-(1H,4H)-吡啶并[1,6]萘啶-1-基)丙-1-胺(8),总收率28%。目标化合物和中间体的结构经1H NMR, 13C NMR和HR-MS确证。
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分别以1-溴萘和酮或1-萘甲醛及有机金属试剂为原料,经12步反应合成了8个含萘三氮唑甲烷骨架的硫代乙酸类尿酸转运体1(URAT1)抑制剂(1h~1o),其结构经1H NMR, 13C NMR和MS(ESI)表征。体外活性测试结果显示:对URAT1的抑制活性最强的是1k,是阳性对照药lesinurad的133倍[IC50=0.054 μmol·L-1(1k), 7.18 μmol·L-1(lesinurad)]。 相似文献
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以2-乙氧基乙胺和3-氯-1-丙醇等为起始原料, 经7步反应, 制备了N,N-二[二(3-甲氧基丙基)膦基乙基]-2-乙氧基乙胺(PNP5)盐酸盐, 其中关键步骤是后两步. PNP5盐酸盐的结构和组成通过IR, 1H NMR, 13C NMR, 31P NMR, MS和元素分析等方法确认. 相似文献
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以4,6-二甲基-2-甲氧基-1,3-苯二甲酸二乙酯为原料,经Micheal加成、环化、溴化、消除等5步反应,合成新型的多取代2,7-萘二甲酸二乙酯.该合成路线步骤少,收率高,反应条件温和.产物中的4个新化合物的结构均经元素分析、核磁共振、红外光谱和质谱确证. 相似文献
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Two types of palladiu m(Ⅱ)-based metallacalixarenes[ML]2+and[ML2]2+have been synthesized through coordination-driven self-assembly from a series of flexible pyridine-bridged diimidazole ligands[2,6-bis((1 H-imidazol-1-yl)methyl)pyridine(L1),2,6-bis((1 H-benzo[d]imidazol-1-yl)methyl)pyridine(L2),2,6-bis((1 H-naphtho[2,3-d]imidazol-1-yl)methyl)pyridine(L3)],with palladium(II)-based building blocks[Pd(BF4)2(M1-BF_4)and(tmeda)Pd(NO3)2(M2-NO3)(tmeda=N,N,N',N'-tetramethyl-ethylenediamine)].All complexes were characterized by NMR spectroscopy(1H NMR and13C NMR),mass spectrometry(CSIMS,ESI-HRMS)and elemental analysis.The single crystal X-ray diffraction analysis of[M1L2_2](NO3)2,[M1L3_2](NO3)2,[M1L3_2](PF_6)_2 and[M~2 L3](NO3)2further confirmed the uniquely single bowl-shape and double bowl-shape structures.The anion binding properties within the metallacalixarenes as receptors were also investigated by NMR titration experiments in DMSO. 相似文献
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E. Grech Z. Malarski W. Sawka-Dobrowolska L. Sobczyk 《Journal of Molecular Structure》1997,416(1-3):227-234
X-Ray diffraction, IR and 1H NMR studies were performed on the 1:1 adduct of 1,8-bis(dimethylamino)naphthalene (DMAN) with 1,8-dihydroxy-2,4-dinitronaphthalene (DHDNN). The adduct crystallizes in the triclinic system, space group
, a = 9.911(2) Å, b = 11.212(2) Å, c = 11.194(2) Å, = 68.95(2)°, β = 79.72(2)°, γ = 73.78(2)°, Z = 2. Both [NHN]+ and [OHO]− hydrogen bonds formed in the ion pairs are asymmetrical with lengths equal to 2.574(2) Å and 2.466(4) Å respectively. The [NHN]+ bridge shows a typical behaviour in the IR spectrum, i.e. a low-frequency absorption between 300 and 700 cm−1. The coupling of [OHO]− hydrogen bonds with the naphthalene π-electron system is so strong that no absorption related to the proton stretching vibrations can be detected in the high- and low-frequency regions. The 1H NMR chemical shifts for the [NHN]+ and [OHO]− bridge protons of 18.63 and 15.81 ppm respectively confirm the strong hydrogen bonds. 相似文献
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Margaret Mwihaki Ng’ang’a Hidayat Hussain Sumesh Chhabra Caroline Langat-Thoruwa Ahmed AI-Harrasi Karsten Krohn Ivan Robert Green 《中国化学快报》2012,23(5):576-578
Two new naphthalene derivatives named eucleanal A and B(1 and 2) were isolated from Euclea divinorum.The structures of the new compounds were elucidated by detailed spectroscopic analysis such as 1H,13C NMR,COSY,HMQC,HMBC and HREIMS mass spectrometry. 相似文献
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Khodayar Gholivand Carlos O. Della Vdova Mauricio F. Erben Fresia Mojahed Ahlam Madani Alizadehgan 《Journal of Molecular Structure》2007,840(1-3):66-70
Using phosphorus pentachloride as a substrate, a new carbacyclamidophosphate, N,N″-bis (2,6-dimethylmorpholino), N″-dichloroacetyl phosphoric triamide (1) has been synthesized and characterized by 1H, 31P and 13C NMR, IR spectroscopy and elemental analysis. Due to the presence of methyl disubstituted morpholine rings and the dichloroacetamide group, several conformers can be considered for this molecule. The 31P{1H} NMR spectra for the isomeric mixture of synthesized compound showed four signals with the ratio 67.1; 19.0; 12.2; 1.7, which indicates four independent conformers. The 1H NMR spectra confirmed these results. The conformational space and the molecular geometry of the molecule in the gaseous phase have been studied using the B3LYP method of approximation, with 6-31G and 6-311++G** basis sets. 相似文献
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Free radical hydrostannation of methyl cyclohexene-1-carboxylate (I) and methyl indene-3-carboxylate (III) with trialkyltin hydrides, R3SnH (R = Me, n-Bu, Ph) gives the energetically unfavourable cis products, 2-trialkylstannyl cyclohexanecarboxylate (II) and 2-trialkylstannyl indane-1-carboxylate (IV) in high yields, via a trans addition of the tin hydrides. The hydride abstractions by the intermediate trialkylstannylcyclohexanyl (VIII) and trialkylstannylindanyl (IX) intermediate radicals take place stereospecifically, and exclusively from the less hindered ring side. The structures of the isomers II and IV were established by (a) their transformation into the corresponding chlorodialkylstannyl derivatives V and VI, which were shown spectroscopically to have cis stereochemistries by intramolecular complexation of the ester group, and (b) their NMR data. Full 1H, 13C, and 119Sn NMR data are given. 相似文献
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合成了一个供体-受体(D-A)型含芘萘啶衍生物2-(芘-1-基)-1,8-萘啶(PN)。 通过核磁共振波谱(NMR)、傅里叶变换红外光谱(FTIR)、液-质联用仪(LC-MS)表征了其结构。 通过电子光谱和Z-扫描技术方法分别研究了化合物PN的线性光学性质和三阶非线性光学吸收,采用综合热分析方法测定了它的热稳定性。 结果表明,在532 nm、180 fs条件下,PN的三阶非线性吸收行为为反饱和吸收,其吸收系数为β=9.0×10-14 m/W,显示出超快三阶非线性光学响应。 运用密度泛函理论方法计算了分子轨道能量、极化率和超极化率,结果表明电子转移能够在分子内部进行。 2-(芘-1-基)-1,8-萘啶的紫外光谱在450 nm以上无吸收,在非线性光学吸收、激光防护、吸收型光开关或双稳器件等方面可作备选材料。 相似文献
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Yuhong Li Xin-Ping Wu Cong Liu Meng Wang Benteng Song Guiyun Yu Gang Yang Wenhua Hou Xue-Qing Gong Luming Peng 《物理化学学报》2020,36(4):1905021-0
Partially reduced TiO2 nanomaterials have attracted significant interest because of their visible-light activity for catalysis and photodegradation. Herein, we prepared a partially reduced anatase TiO2 (Re-A-TiO2) nanoparticle material using a fast combustion method, demonstrating good activity toward decomposing methyl orange under visible light irradiation. The surface structure of the prepared material, after being surface-selectively 17O-labeled with H217O (17O-enriched water), was studied via 17O and 1H solid-state magic angle spinning nuclear magnetic resonance (MAS NMR) spectroscopy and electron paramagnetic resonance (EPR) spectroscopy, and the obtained results were compared to those of non-reduced anatase TiO2 (A-TiO2). The EPR results showed that the concentrations of paramagnetic species (i.e., oxygen vacancies (OV) and Ti3+) in Re-A-TiO2 were much higher than that in A-TiO2, while the former was associated with a higher OV/Ti3+ ratio. The intensities of the EPR signals were significantly affected by the adsorbed water, and this phenomenon was explored in combination with 1H NMR spectroscopy. The 1H species on Re-A-TiO2 appeared at larger chemical shifts, denoting the increased acidity of the sample, and these 1H species on Re-A-TiO2 were more difficult to remove than those on A-TiO2. On the other hand, different features were observed for the signals arising from the two-coordinated oxygen atoms (μ2-O) in 17O NMR, suggesting a typical anatase TiO2(101) surface on A-TiO2, but a more complex surface environment for Re-A-TiO2. Furthermore, a larger amount of hydroxyl groups (OH) were observed on Re-A-TiO2 compared to that on A-TiO2, indicating a larger proportion of exposed (001) facets on Re-A-TiO2. However, the μ2-O signals broadened and became similar when the drying temperature was increased to 100 ℃, indicating a non-faceted anatase TiO2 surface in such conditions. Based on the EPR and NMR results, a significant fraction of the OH species is believed to be formed from the reaction of the paramagnetic centers and adsorbed water molecules. The 1H→17O cross polarization (CP) MAS and two-dimensional heteronuclear correlation (2D HETCOR) NMR spectra were used to verify the spatial proximity of the hydrogen and oxygen species, confirming the spectral assignments of a strongly adsorbed water and one type of surface OH species. In particular, the 1H NMR signals at approximately 11 ppm were ascribed to the hydrogen species in the intramolecular hydrogen bond. In summary, this study investigated the paramagnetic species and surface structure of anatase TiO2 materials by combining EPR along with 1H and 17O solid-state NMR spectroscopy. The differences in the surface structures of Re-A-TiO2 and A-TiO2 should be closely related to their different properties toward the photodegradation of methyl orange. 相似文献
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Vadim V. Negrebetsky Aleksandr G. Shipov Evgeniya P. Kramarova Vitaliy V. Negrebetsky Yuri I. Baukov 《Journal of organometallic chemistry》1997,530(1-2):1-12
The structure and dynamic behavior of (O-Si)-chelate N-(dimethylhalogenosilyl)methyl acetamides of the type MeC(O)N(CH(Ph)Me)CH2 SiMe2 X, where X = F, Cl, Br with the OSiC3X coordination set, were studied by multinuclear (1H, 13C, 17O, 29Si) and dynamic 1H NMR spectroscopy. Ligand permutation at silicon was detected. The observed influence of the solvent, nucleofugacity of the X substituent and the external nucleophile on the calculated values of the free energies of activation testify to the dissociative and/or associative mechanisms of the process, but including the stages in which the regular (pseudo-rotation or ‘turnstile’) mechanism takes place. At lower temperatures (up to −90°C) the 1H, 13C, 29Si NMR spectra of N-(dimethylchlorosilyl)methyl acetamide contain the signals of two species of unequal intensity. This effect was explained by an equilibrium between monomers containing the intramolecular O → Si bond and dimers with a hexacoordinate silicon and the bridging chlorine atoms. 相似文献
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以白杨素为起始原料, 通过卤代和水解反应制得中间产物7-O-羧烷基化的白杨素衍生物(6~9); 然后以1-乙基-3-(3-二甲氨基丙基)碳二亚胺(EDCI)、 1-羟基苯并三氮唑(HOBt)和4-二甲氨基吡啶(DMAP)为催化体系, 4个中间产物分别与甘氨酸甲酯盐酸盐进行酰胺缩合反应, 制得白杨素甘氨酸甲酯类化合物12~15; 化合物12~15在pH=10~11和室温下水解得到相应的白杨素甘氨酸类化合物(16~19). 所有目标化合物的结构均经 1H NMR, 13C NMR, IR以及MS确认. 以顺铂为阳性对照药物, 采用噻唑蓝比色(MTT)法检测了目标化合物对人肝癌细胞HepG2和人胃癌细胞MGC-803的体外增殖抑制作用. 结果表明, 目标化合物14~16, 18和19的体外抗肿瘤活性明显强于白杨素, 且化合物18(IC50=4.36 μmol/L)对MGC-803细胞的增殖抑制作用强于阳性药物顺铂(IC50=4.40 μmol/L). 相似文献