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用一维1H、13C NMR谱、DEPT 13C NMR谱、选择性远程DEPT 13C NMR、1H-1H COSY和13C-1H COSY二维核磁共振技术研究了南海海绵Dysidea fragilis中的两个倍半萜herbadysidolide(1)和furodysinin lactone(2),确认了化学结构,并对其13C NMR和1H NMR谱进行了归属.药理活性试验表明:1和2具有一定的心血管活性. 相似文献
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南蛇藤中倍半萜生物碱的二维NMR研究 总被引:1,自引:0,他引:1
用DEPT和二维NMR技术包括:1H-1H COSY,1H-13C COSY,NOESY,特别是1H-13C COLOC对两个多酯基取代的倍半萜生物碱的化学及立体结构进行了研究,并对其1H和13C NMR谱峰进行了归属。 相似文献
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滇黄精中两个呋甾皂苷的NMR研究 总被引:1,自引:0,他引:1
从滇黄精新鲜根茎中分离得到一对立体异构的呋甾皂苷, 利用1D、2D NMR鉴定其结构为: 26-O-β-D-吡喃葡萄糖基25(S)-呋甾-△5(6)-烯-3β, 22, 26-三羟基-12酮基-3-O-β-D-吡喃葡萄糖基(1→4)-β-D-吡喃呋糖苷(1, 25S-kingianoside D)和26-O-β-D-吡喃葡萄糖基25(R)-呋甾-△5(6)-烯-3β-, 22, 26-三羟基-12酮基-3-O-β-D-吡喃葡萄糖基(1→4)-β-D-吡喃呋糖苷(2, kingianoside D). 利用1D、2D NMR对两个呋甾皂苷25位的立体构型进行了确定, 并对其碳、氢信号进行了全归属. 相似文献
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对3′″-羰基-2″-β-L-奎诺糖基淫羊藿次苷Ⅱ(3′″-carbonyl-2″-β-L-quinovosyl icariside Ⅱ),进行了1H和13C MNR检测,参考2″-O-鼠李糖基淫羊藿次苷Ⅱ (2″-O-rhamnosyl icarisid Ⅱ)、淫羊藿次苷Ⅱ(icarisid Ⅱ)和淫羊藿苷(icariin)的1H、13C NMR数据,通过DEPT和1H-1H COSY、HSQC、HMBC等2D NMR技术对该化合物所有的1H和13C NMR信号进行了全归属和详细解析. 相似文献
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The complete structural analysis of 1-[(4-methoxyphenyl)-(3,4,5-trimethoxyphe- nyl)methyl]naphtalene 5a and 1-[(2,5-dimethoxyphenyl)-(3,4,5-trimethoxyphenyl) methyljnaphtalene 5b, prepared by alkylation of 1-[chloro-(3,4,5-trimethoxyphenyl) methyl]naphtalene without by-products such as benzofluorene 2, may be accurately determined by 1H, 13C NMR and 2D NMR analysis. 相似文献
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Mansoureh Mousavi Steve S.-F. Yu Der-Lii M. Tzou 《Solid state nuclear magnetic resonance》2009,36(1):24-31
13C cross-polarization/magic-angle spinning (CP/MAS) solid-state NMR spectroscopy has been employed to analyze four vitamin D compounds, namely vitamin D3 (D3), vitamin D2 (D2), and the precursors ergosterol (Erg) and 7-dehydrocholesterol (7DHC). The 13C NMR spectrum of D3 displays a doublet pattern for each of the carbon atoms, while that of Erg contains both singlet and doublet patterns. In the cases of 7DHC and D2, the 13C spectra display various multiplet patterns, viz. singlets, doublets, triplets, and quartets. To overcome the signal overlap between the 13C resonances of protonated and unprotonated carbons, we have subjected these vitamin D compounds to 1D 1H-filtered 13C CP/MAS and {1H}/13C heteronuclear correlation (Hetcor) NMR experiments. As a result, assisted by solution NMR data, all of the 13C resonances have been successfully assigned to the respective carbon atoms of these vitamin D compounds. The 13C multiplets are interpreted due to the presence of s-cis and s-trans configurations in the α- and β-molecular conformers, consistent with computer molecular modeling determined by molecular dynamics and energy minimization calculations. To further characterize the ring conformations in D3, we have successfully extracted chemical shift tensor elements for the 13C doublets. It is demonstrated that 13C solid-state NMR spectroscopy provides a robust and high sensitive means of characterizing molecular conformations in vitamin D compounds. 相似文献
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由D-木糖出发,经过杂D-A 反应、Henry反应、合成了中间体(1αS,2αR, 3αS,4S,7E,9αR,10αR)-1,2∶9,10-O-二异丙叉基-3-硝甲基-5,6-二脱氧-7-烯-4-氧化-1,4∶7,10-二呋喃-4,8-吡喃糖(化合物1),再经催化氢化,立体选择性地得到了含高碳糖结构片断的β-氨基醇(1αS,2αR, 3αS,4S,7αS,8βR,9αR,10αR)-1,2∶9,10-O-二异丙叉基-3-氨甲基-5,6-二脱氧-4-氧化-1,4∶7,10-二呋喃-4,8-吡喃糖(化合物2), 通过DEPT和1H-1H COSY,HMQC,HMBC等2D NMR 技术对化合物1的1H和13C NMR数据进行了全归属和较详细的解析并探讨了其ESI-MS/MS质谱裂解规律. 同时得到化合物1的还原产物化合物2的1H,13C NMR归属. 相似文献
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The potent Diels-Alder diene, phencyclone, 1, reacts with N-pentafluorophenylmaleimide, 2, to form an adduct, 3, characterized by 1H, 13C, and 19F NMR at 300, 75 and 282 MHz, respectively. The one-dimensional (1D) and two-dimensional (2D) 1H and 13C NMR spectra of 3 at ambient temperatures imply a slow exchange limit (SEL) regime with respect to rotation of the unsubstituted bridgehead phenyl groups about severely hindered C(sp2)-C(sp3) bonds. Major non-bonded interactions are expected between the ortho protons of the C6H5 groups and H-1, 8 of the phenanthrenoid moiety of 3. 19F 1D and 2D (COSY) NMR spectra show that the SEL regime also obtains for rotation about the N-C6F5 bond of 3, with five separate fluorine signals seen, consistent with a preferred conformation in which the C6F5 may lie roughly perpendicular to the plane of the pyrrolidinedione moiety, and may be in the mirror symmetry plane of 3. The results are considered relevant to hindered aryl rotations in numerous Pharmaceuticals. Selected spectral data for 2 and precursors are also presented. 相似文献
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A complete assignment of the two dimensional 1H and 13C NMR spectra of the title compound, which is a key intermediate for preparation of podophyllotoxin derivatives, is presented The proton signals have been assigned from DQF-COSY, TOCSY, 1H-1H coupling patterns, and by the comparisons of chemical shifs with those of similar podophyllum lignans. Complete 13C NMR assignments have been made from HMQC.HMBC and DEPT spectra. Further information on the stereochemistry of the molecule was obtained from 2D NOESY and NOE-difference techniques. 相似文献