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1.
Simona Hybelbauerová Jan Sejbal Martin Dračínský Iva Rudovská Bohumír Koutek 《Helvetica chimica acta》2009,92(12):2795-2801
The two previously unreported esters 1 and 2 of pentane‐2,4‐diol and p‐coumaric acid (=3‐(4‐hydroxyphenyl)prop‐2‐enoic acid) along with 13 known compounds including 6 oleanane‐ and ursane‐type triterpenoids were isolated from MeOH extracts of the stems of Vaccinium myrtillus. The structures of the new compounds were assigned as (2S,4R)‐4‐(β‐D ‐glucopyranosyloxy)pentan‐2‐yl (2E)‐p‐coumarate ( 1 ) and its aglycone 2 on the basis of 1D‐ and 2D‐NMR spectroscopic analyses of the isolated and synthesized compounds and molecular modelling experiments. This is the first report on the occurrence of a chiral pentane‐2,4‐diol linker between the phenol‐derived acid and a glycoside part in natural products. 相似文献
2.
Najeeb Ur Rehman Abdul Latif Khan Zahid Hassan Tania Shamim Rizvi Ahmed Al‐Harrasi Zabta Khan Shinwari Javid Hussain 《Helvetica chimica acta》2015,98(9):1240-1244
One new cyclopropyl‐triterpenoid ( 1 ), along with four known constituents including octacosan‐1‐ol ( 2 ), pentacosanoic acid ( 3 ), β‐sitosterol ( 4 ), and β‐sitosterol 3‐O‐β‐D ‐glucopyranoside ( 5 ) were isolated from the aerial parts of Ochradenus arabicus for the first time. These compounds were isolated by repeated column chromatography followed by further purification through recycling HPLC. The structure of the new secondary metabolite 1 was established on the basis of UV, IR, 1D‐ (1H‐ and 13C‐) and 2D‐NMR (HMBC and HSQC), and MS spectral data. The molecular mass was determined by HR‐MS, and hence the molecular formula was deduced. The configurations of stereogenic centers in the molecule were assigned by NOESY experiments, along with biogenetic considerations. The structures of the known compounds were confirmed by comparison of their physical and spectroscopic data with those reported in literature. 相似文献
3.
Chang‐Ming Dong Kun‐Yuan Qiu Zhong‐Wei Gu Xin‐De Feng 《Journal of polymer science. Part A, Polymer chemistry》2002,40(3):409-415
Two types of three‐arm and four‐arm, star‐shaped poly(D,L ‐lactic acid‐alt‐glycolic acid)‐b‐poly(L ‐lactic acid) (D,L ‐PLGA50‐b‐PLLA) were successfully synthesized via the sequential ring‐opening polymerization of D,L ‐3‐methylglycolide (MG) and L ‐lactide (L ‐LA) with a multifunctional initiator, such as trimethylolpropane and pentaerythritol, and stannous octoate (SnOct2) as a catalyst. Star‐shaped, hydroxy‐terminated poly(D,L ‐lactic acid‐alt‐glycolic acid) (D,L ‐PLGA50) obtained from the polymerization of MG was used as a macroinitiator to initiate the block polymerization of L ‐LA with the SnOct2 catalyst in bulk at 130 °C. For the polymerization of L ‐LA with the three‐arm, star‐shaped D,L ‐PLGA50 macroinitiator (number‐average molecular weight = 6800) and the SnOct2 catalyst, the molecular weight of the resulting D,L ‐PLGA50‐b‐PLLA polymer linearly increased from 12,600 to 27,400 with the increasing molar ratio (1:1 to 3:1) of L ‐LA to MG, and the molecular weight distribution was rather narrow (weight‐average molecular weight/number‐average molecular weight = 1.09–1.15). The 1H NMR spectrum of the D,L ‐PLGA50‐b‐PLLA block copolymer showed that the molecular weight and unit composition of the block copolymer were controlled by the molar ratio of L ‐LA to the macroinitiator. The 13C NMR spectrum of the block copolymer clearly showed its diblock structures, that is, D,L ‐PLGA50 as the first block and poly(L ‐lactic acid) as the second block. © 2001 John Wiley & Sons, Inc. J Polym Sci Part A: Polym Chem 40: 409–415, 2002 相似文献
4.
Silvia Capacchi Milco Lipreri Andrea Rizzi Claudia Caló Tiziana Peveri Silvia Catinella 《Magnetic resonance in chemistry : MRC》2009,47(7):551-561
Two diastereoisomers CHF4226.01 (R, R) and CHF4232.01 (S, R), differing for a chiral center, have been studied to investigate their possible discrimination using NMR. 1D NMR and 2D NMR experiments, such as COSY, NOESY and ROESY, were performed on pure isomers and on the association complexes formed in the presence of the chiral reagent (S)‐(?)‐1‐(2‐napthyl)ethylamine (S‐NEA). Moreover, computational studies, concerning conformational analysis and molecular dynamics, were started and supported the NMR results. Copyright © 2009 John Wiley & Sons, Ltd. 相似文献
5.
The phytochemical investigation of the aerial parts of Siegesbeckia pubescens L. yielded 16 sesquiterpenoids, including a novel 11(7→6)abeo‐14‐norcarabrane sesquiterpenoid, pubescone ( 1 ), and a new germacrane sesquiterpene, 5 . The molecular structures of the isolated compounds were elucidated on the basis of extensive spectroscopic analysis, including 1D‐ and 2D‐NMR. 相似文献
6.
Cheng‐Jian Tan Ping Yi Masuo Goto Susan L. Morris‐Natschke Li‐Na Liu Kuo‐Hsiung Lee Bao‐Yu Zhao 《Helvetica chimica acta》2016,99(3):225-227
A new matrine alkaloid derivative (+)‐(14β)‐14‐ethylmatridin‐15‐one ( 1 ) was isolated from the poisonous plant Oxytropis ochrocephala Bunge . The structure was established by spectroscopic methods, including extensive 1D‐ and 2D‐NMR experiments. 相似文献
7.
Highly Efficient Chiral Resolution of dl‐Arginine by Cocrystal Formation Followed by Recrystallization under Preferential‐Enrichment Conditions
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Dr. Sekai Iwama Kazunori Kuyama Yuko Mori Dr. Kochunnoonny Manoj Dr. Rajesh G. Gonnade Dr. Katsuaki Suzuki Dr. Colan E. Hughes P. Andrew Williams Prof. Kenneth D. M. Harris Dr. Stéphane Veesler Dr. Hiroki Takahashi Prof. Hirohito Tsue Prof. Rui Tamura 《Chemistry (Weinheim an der Bergstrasse, Germany)》2014,20(33):10343-10350
An excellent chiral symmetry‐breaking spontaneous enantiomeric resolution phenomenon, denoted preferential enrichment, was observed on recrystallization of the 1:1 cocrystal of dl ‐arginine and fumaric acid, which is classified as a racemic compound crystal with a high eutectic ee value (>95 %), under non‐equilibrium crystallization conditions. On the basis of temperature‐controlled video microscopy and in situ time‐resolved solid‐state 13C NMR spectroscopic studies on the crystallization process, a new mechanism of phase transition that can induce preferential enrichment is proposed. 相似文献
8.
Stephanie A. Kingsbury Curtis J. Ducommun Bryan M. Zahakaylo Elizabeth H. Dickinson Kevin F. Morris 《Magnetic resonance in chemistry : MRC》2010,48(3):184-191
NMR spectroscopy was used to characterize the binding of the chiral compound 1,1′‐binaphthyl‐2,2′‐diyl hydrogen phosphate (BNP) to five molecular micelles with chiral dipeptide headgroups. Molecular micelles have covalent linkages between the surfactant monomers and are used as chiral mobile phase modifiers in electrokinetic chromatography. Nuclear overhauser enhancement spectroscopy (NOESY) analyses of (S)‐BNP:molecular micelle mixtures showed that in each solution the (S)‐BNP interacted predominately with the N‐terminal amino acid of the molecular micelle's dipeptide headgroup. NOESY spectra were also used to generate group binding maps for (S)‐BNP:molecular micelle mixtures. In these maps, percentages are assigned to the (S)‐BNP protons to represent the relative strengths of their interactions with a specified molecular micelle proton. All maps showed that (S)‐BNP inserted into a previously reported chiral groove formed between the molecular micelle's dipeptide headgroup and hydrocarbon chain. In the resulting intermolecular complexes, the (S)‐BNP protons nearest to the analyte phosphate group were found to point toward the N‐terminal Hα proton of the molecular micelle headgroup. Finally, pulsed field gradient NMR diffusion experiments were used to measure association constants for (R) and (S)‐BNP binding to each molecular micelle. These K values were then used to calculate the differences in the enantiomers' free energies of binding, Δ(ΔG). The NMR‐derived Δ(ΔG) values were found to scale linearly with electrokinetic chromatography (EKC) chiral selectivities from the literature. Copyright © 2010 John Wiley & Sons, Ltd. 相似文献
9.
Jyh‐Horng Wu Yi‐Fu Chang Yu‐Tang Tung Minoru Tsuzuki Akira Izuka Sheng‐Yang Wang Yueh‐Hsiung Kuo 《Helvetica chimica acta》2010,93(4):753-756
Two novel 15(10→1)abeomuurolane sesquiterpenes, cosmosoic acid ( 1 ) and cosmosaldehyde ( 2 ), were isolated from the whole plant of Cosmos sulfurous. Their structures were established by a combination of 1D‐ and 2D‐NMR spectroscopic techniques. Additionally, a chemical correlation between 1 and 2 was also established. 相似文献
10.
Amadou Dawe Gilbert Deccaux Wabo Fotso Kapche Jean Jules Kezetas Bankeu Yakai Fawai Muhammad Shaiq Ali Bonaventure Tchaleu Ngadjui 《Helvetica chimica acta》2016,99(8):617-620
The phytochemical studies on the leaves of the traditionally used medicinal plant Combretum fragrans F. Hoffm (Combretaceae) from Cameroon have led to the isolation of combretins A and B ( 1 and 2 , resp.), two new cycloartane‐type triterpenes from the AcOEt‐soluble subfraction along with β‐sitosterol ( 3 ), oleanolic acid ( 4 ), ursolic acid ( 5 ), and pratensein ( 6 ). The compounds 4 – 6 are reported for the first time from this species. The structures of the new triterpenes were elucidated by spectroscopic techniques including 1H‐ and 13C‐NMR (DEPT), and 2D‐NMR experiments. 相似文献
11.
Qifang Tan Xuefen Yan Xiang Lin Yaojian Huang Zhonghui Zheng Siyang Song Chunhua Lu Yuemao Shen 《Helvetica chimica acta》2007,90(9):1811-1817
From the endophytic fungal strain Phomopsis sp. NXZ‐05 of Camptotheca acuminata Decne . (Nyssaceae), six new compounds were isolated, including the ten‐membered macrolides 1 – 4 and their (known) parent compound multiplolide A ( 7 ), as well as a new unsaturated fatty acid, (4E)‐6,7,9‐trihydroxydec‐4‐enoic acid ( 5 ) and its methyl ester 6 . Their structures were elucidated by spectroscopic and mass‐spectrometric analyses, including 1D‐ and 2D‐NMR experiments and HR‐ESI‐MS, and their biological activities were elucidated. 相似文献
12.
《Magnetic resonance in chemistry : MRC》2002,40(9):603-608
Four new ursane‐type saponins, monepalosides C–F, together with a known saponin, mazusaponin II, were isolated from Morina nepalensis var. alba Hand.‐Mazz. Their structures were determined to be 3‐O‐α‐L ‐arabinopyranosyl‐(1 → 3)‐&[alpha;‐L ‐rhamnopyranosyl‐(1 → 2)]‐α‐L ‐arabinopyranosylpomolic acid 28‐O‐β‐D ‐glucopyranosyl‐(1 → 6)‐β‐D ‐glucopyranoside (monepaloside C, 1 ), 3‐O‐α‐L ‐arabinopyranosyl‐(1 → 3)‐&[alpha;‐L ‐rhamnopyranosyl‐(1 → 2)]‐β‐D ‐xylopyranosylpomolic acid 28‐O‐β‐D ‐glucopyranosyl‐(1 → 6)‐β‐D ‐glucopyranoside (monepaloside D, 2 ), 3‐O‐α‐L ‐arabinopyranosyl‐(1 → 3)‐&[beta;‐D ‐glucopyranosy‐(1 → 2)]‐α‐L ‐arabinopyranosylpomolic acid 28‐O‐β‐D ‐glucopyranosyl‐(1 → 6)‐β‐D ‐glucopyranoside (monepaloside E, 3 ) and 3‐O‐β‐D ‐xylopyranosylpomolic acid 28‐O‐β‐D ‐glucopyranoside (monepaloside F, 4 ) on the basis of chemical and spectroscopic evidence. 2D NMR techniques, including 1H–1H COSY, HMQC, 2D HMQC‐TOCSY, HMBC and ROESY, and selective excitation experiments, including SELTOCSY and SELNOESY, were utilized in the structure elucidation and complete assignments of 1H and 13C NMR spectra. Copyright © 2002 John Wiley & Sons, Ltd. 相似文献
13.
Yun‐Chih Lin Dr. Hung‐Lung Chou Dr. Loka Subramanyam Sarma Dr. Bing‐Joe Hwang Prof. 《Chemistry (Weinheim an der Bergstrasse, Germany)》2009,15(40):10658-10665
Understanding the complex thermodynamic behavior of confined amphiphilic molecules in biological or mesoporous hosts requires detailed knowledge of the stacking structures. Here, we present detailed solid‐state NMR spectroscopic investigations on 1‐butanol molecules confined in the hydrophilic mesoporous SBA‐15 host. A range of NMR spectroscopic measurements comprising of 1H spin–lattice (T1), spin–spin (T2) relaxation, 13C cross‐polarization (CP), and 1H,1H two‐dimensional nuclear Overhauser enhancement spectroscopy (1H,1H 2D NOESY) with the magic angle spinning (MAS) technique as well as static wide‐line 2H NMR spectra have been used to investigate the dynamics and to observe the stacking structure of confined 1‐butanol in SBA‐15. The results suggest that not only the molecular reorientation but also the exchange motions of confined molecules of 1‐butanol are extremely restricted in the confined space of the SBA‐15 pores. The dynamics of the confined molecules of 1‐butanol imply that the 1H,1H 2D NOESY should be an appropriate technique to observe the stacking structure of confined amphiphilc molecules. This study is the first to observe that a significant part of confined 1‐butanol molecules are orientated as tilted bilayered structures on the surface of the host SBA‐15 pores in a time‐average state by solid‐state NMR spectroscopy with the 1H,1H 2D NOESY technique. 相似文献
14.
One novel p‐terphenyl compound, named vialisyl A ( 1 ), was isolated from the fruiting bodies of Thelephora vialis, together with six known compounds, ganbajunin B ( 2 ), phenylacetic acid ( 3 ), a mixture of ganbajunins D ( 4 ) and E ( 5 ), and vialinins A ( 6 ) and B ( 7 ). Their structures were established by extensive analysis of spectroscopic data (including 1H‐ and 13C‐NMR, HSQC, HMBC, 2D‐INADEQUATE) as well as by comparison with literature reports. 相似文献
15.
Molecular Recognition of α,α,α,β-ZnT(o-BocThr)APP (1) toward a series of imidazole derivatives and amino acid esters was investigated. Association constants were determined in chloroform by means of UV-Vis titration method. The association constants of 1 with imidazole derivatives are larger than those of 1 with amino acid esters. 1H NMR spectra were investigated to describe the binding mode of the recognition system, showing that all the protons of the guests were shifted to upfield. The circular dichroism spectra of 1-L-/D-ValOMe showed a split cotton effect in Soret region, while those of 1-L-/D-PheOMe showed no split cotton effect. Molecular modeling was performed to understand chiral recognition on a molecular level. Quantum chemical calculation was carried out based on the stable conformations of these recognition systems, which gave a reasonable explanation for the behavior of molecular recognition. The results indicated that the conformation of 1-D-ValOMe was more stable than that of 1-L-ValOMe. 相似文献
16.
Valerie Huemer Gernot A. Eller Wolfgang Holzer 《Magnetic resonance in chemistry : MRC》2010,48(6):476-482
Various [5,6]pyrano[2,3‐c]pyrazol‐4(1H)‐thiones were synthesized in high yields by treatment of the corresponding [5,6]pyrano[2,3‐c]pyrazol‐4(1H)‐ones with Lawesson's reagent. Detailed NMR spectroscopic studies were undertaken of the title compounds. Complete and unambiguous assignment of chemical shifts (1H, 13C, 15N) and coupling constants (1H,1H; 13C,1H) was achieved by the combined application of various one‐ and two‐dimensional (1D and 2D) NMR spectroscopic techniques. Unequivocal mapping of most 13C,1H spin coupling constants is accomplished by 2D (δ, J) long‐range INEPT spectra with selective excitation. Copyright © 2010 John Wiley & Sons, Ltd. 相似文献
17.
Chang‐Ming Dong Kun‐Yuan Qiu Zhong‐Wei Gu Xin‐De Feng 《Journal of polymer science. Part A, Polymer chemistry》2001,39(3):357-367
D,L ‐3‐Methylglycolide (MG) was successfully polymerized with bimetallic (Al/Zn) μ‐oxo alkoxide as an initiator in toluene at 90 °C. The effect of the initiator concentration and monomer conversion on the molecular weight was studied. It is shown that the polymerization of MG follows a living process. A kinetic study indicated that the polymerization approximates the first order in the monomer, and no induction period was observed. 1H NMR spectroscopy showed that the ring‐opening polymerization proceeds through a coordination–insertion mechanism with selective cleavage of the acyl–oxygen bond of the monomer. On the basis of 1H NMR and 13C NMR analyses, the selective cleavage of the acyl–oxygen bond of the monomer mainly occurs at the least hindered carbonyl groups (P1 = 0.84, P2 = 0.16). Therefore, the main chain of poly(D,L ‐lactic acid‐co‐glycolic acid) (50/50 molar ratio) obtained from the homopolymerization of MG was primarily composed of alternating lactyl and glycolyl units. The diblock copolymers poly(ϵ‐caprolactone)‐b‐poly(D,L ‐lactic acid‐alt‐glycolic acid) and poly(L ‐lactide)‐b‐poly(D,L ‐lactic acid‐alt‐glycolic acid) were successfully synthesized by the sequential living polymerization of related lactones (ϵ‐caprolactone or L ‐lactide). 13C NMR spectra of diblock copolymers clearly show their pure diblock structures. © 2000 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 39: 357–367, 2001 相似文献
18.
Hai‐Tao Xiao Xiao‐Yan Hao Xian‐Wen Yang Yue‐Hu Wang Yang Lu Ying Zhang Suo Gao Hong‐Ping He Xiao‐Jiang Hao 《Helvetica chimica acta》2007,90(1):164-170
A novel bisabolane‐type sesquiterpenoid lactone, glochicoccin A ( 1 ), and three new norbisabolane sesquiterpenoids, glochicoccins B–D ( 2 – 4 ), together with two known norbisabolane sesquiterpenoids, phyllaemblic acid ( 5 ) and phyllaemblic acid methyl ester ( 6 ), were isolated from the rhizomes of Glochidion coccineum. Their structures were elucidated by different spectroscopic (IR, UV, NMR) and mass‐spectrometric (MS) techniques. The structure and relative configuration of 1 was confirmed by single‐crystal X‐ray diffraction (Fig. 2). None of the compounds were found to exhibit cytotoxic or antioxidant activities. 相似文献
19.
Two new and a known N‐(O‐carbamoylglucopyranosyl)ansamitocins were isolated from Actinosynnema pretiosum ssp. auranticum ATCC 31565. The known N‐(4‐O‐carbamoyl‐β‐D ‐glucopyranosyl)‐N‐demethylansamitocin P 2 (=ACGP‐2; 1 ) was assigned according to 1D‐ and 2D‐NMR data, and the two new compounds were identified as N‐(6‐O‐carbamoyl‐β‐D ‐glucopyranosyl)‐N‐demethylansamitocin P 2 (=ACGP‐2′; 2 ) and N‐(4‐O‐carbamoyl‐β‐D ‐glucopyranosyl)‐N‐demethylansamitocin P 1 (=ACGP‐1; 3 ) on the basis of spectroscopic data interpretation including 2D‐NMR and tandem MS analysis. 相似文献
20.
You‐Xing Zhao Cheng‐Sen Li Xiao‐Dong Luo Tie‐Mei Yi Jun Zhou 《Helvetica chimica acta》2005,88(2):325-329
Three new urea derivatives, isolated from the Pliocene lignified wood of Pinus armandii, were identified as carbonylbis[imino(6‐methyl‐3,1‐phenylene)]bis[carbamic acid] dimethyl ester ( 1 ), and as the corresponding dibutyl ester 2 and bis(2‐methylpropyl) ester 3 . Their structures were elucidated by spectroscopic methods, including MS and 1D‐ and 2D‐NMR techniques. 相似文献