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1.
E. A. Khamidullina A. S. Gromova V. I. Litskii A. L. Vereshchagin A. A. Semenov M. F. Larin 《Chemistry of Natural Compounds》1989,25(4):441-447
Four new cycloartane glycosides have been isolated from a methanolic extract ofThalictrum squarrosum Stephan ex Willd.: squarroside A1 (I) — (21R, 22S, 23R)-3β-(β-D-glucopyranosyloxy)-21α-methoxy-21,23-epoxycycloart-24-ene-22β,30-diol,
C30H60O10; squarroside A2 (II) — the (21S)-epimer of compound (I); squarroside B1 (III) (21R, 22S, 23R)-3gb-[O-α-L-rhamnopyranosyl-(1
→ 6)-β-D-glucopyranosyloxy]-21α-methoxy-21,23-epoxycycloart-24-ene-22β,30-diol, C43H70O14; and squarroside B2 (IV) — the (21S)-epimer of compound (III). The proposed structures were determined on the basis of1H and13C NMR spectroscopy, FAB mass spectrometry, and chemical transformations.
Irkutsk Institute of Organic Chemistry, Siberian Branch, USSR Academy of Sciences. Translated from Khimiya Prirodnykh Soedinenii,
No. 4, pp. 516–523, July–August, 1989. 相似文献
2.
M. Vorona I. Potoročina G. Veinberg I. Shestakova I. Kanepe M. Petrova E. Liepinsh E. Lukevics 《Chemistry of Heterocyclic Compounds》2007,43(5):646-652
The reaction of tert-butyl 7α-chloro-and 7-β-chloro-7α-isopropoxy-3-methyl-1,1-dioxoceph-3-em-4-carboxylates with the Vilsmeier
reagent was carried out with introduction of N,N-dimethylaminomethylene group at position 2 in the E-and Z-isomeric forms.
Prolonged treatment of tert-butyl 7α-chloro-3-methyl-2-(N,N-dimethylaminomethylene)-1,1-dioxoceph-3-em-4-carboxylate with
hydroxylamine hydrochloride in acetonitrile at 40–50°C gave tert-butyl 10(S)-chloro-6-methyl-5-oxa-1,1,9-trioxo-1-thia-4,8-diazatricyclo[7,2,0,02,6]undecane-7(R)-carboxylate which isomerized into 1-tertbutoxycarbonylmethyl-3α-chloro-4-(5-methylisoxazole-4-sulfonyl)azetidin-2-one.
In the case of tertbutyl 7β-chloro-7α-isopropoxy-3-methyl-2-(N,N-dimethylaminomethylen)-1,1-dioxoceph-3-em-4-carboxylate the
analogous reaction gave tert-butyl 10β-chloro-(2S,6S,7S,10R,11R)-10α-isopropoxy-6-methyl-5-oxa-1,1,9-trioxo-1-thia-4,8-diazatricyclo[7,2,0,02,6]undecane-7(R)-carboxylate, the struc-ture of which was determined by 2D-NOESY two-dimensional spectroscopy. The compounds
synthesized showed weak or no cytotoxic activity with respect to monolayers of cancer cells in vitro. 相似文献
3.
Determination of the structure of heparin-derived oligosaccharides by 1H NMR is challenging because resonances for all but the anomeric protons cover less than 2 ppm. By taking advantage of increased
dispersion of resonances for the anomeric H1 protons at low pD and the superior resolution of band-selective, homonuclear-decoupled (BASHD) two-dimensional 1H NMR, the primary structure of the heparin-derived octasaccharide ∆UA(2S)-[(1 → 4)-GlcNS(6S)-(1 → 4)-IdoA(2S)-]3-(1 → 4)-GlcNS(6S) has been determined, where ∆UA(2S) is 2-O-sulfated ∆4,5-unsaturated uronic acid, GlcNS(6S) is 6-O-sulfated, N-sulfated β-d-glucosamine and IdoA(2S) is 2-O-sulfated α-l-iduronic acid. The spectrum was assigned, and the sites of N- and O-sulfation and the conformation of each uronic acid residue were established, with chemical shift data obtained from BASHD-TOCSY
spectra, while the sequence of the monosaccharide residues in the octasaccharide was determined from inter-residue NOEs in
BASHD-NOESY spectra. Acid dissociation constants were determined for each carboxylic acid group of the octasaccharide, as
well as for related tetra- and hexasaccharides, from chemical shift–pD titration curves. Chemical shift–pD titration curves
were obtained for each carboxylic acid group from sub-spectra taken from BASHD-TOCSY spectra that were measured as a function
of pD. The pK
As of the carboxylic acid groups of the ∆UA(2S) residues are less than those of the IdoA(2S) residues, and the pK
As of the carboxylic acid groups of the IdoA(2S) residues for a given oligosaccharide are similar in magnitude. Relative acidities
of the carboxylic acid groups of each oligosaccharide were calculated from chemical shift data by a pH-independent method. 相似文献
4.
P. Madhavan B. M. Rao Pravin Abhishek P. R. Kumar M. Sreenivasulu K. B. Chandrasekhar 《Chromatographia》2007,65(1-2):81-84
A normal phase chiral LC method for chiral purity evaluation of β-amino-β-(4-methoxyphenyl) propionic acid was developed on
donor–acceptor (pirkle) column. The chiral stationary phase used was a 250 × 4.6 mm (R, R) Whelk-01 with 5 μm particle size,
which was accompanied with a 1 cm long guard column. The “hybrid” pi-electron donor–acceptor based stationary phase (R, R)
Whelk-01 was found to be enantiomeric selective for (R) and (S) enantiomers of β-amino-β-(4-methoxyphenyl) propionic acid
with a resolution >2.5. The concentration of 2-propanol and TFA in the mobile phase plays an important role on the chrmatographic
efficiency and resolution between the enantiomers. The limit of detection and limit of quantification of (S) enantiomer was
0.3 and 1.0 μg mL-1 for 20 μL injection volume. The percentage RSD of the peak area of six replicate injections of (S) enantiomer at LOQ concentration
was 4.5. The percentage recovery of (S) enantiomer from (R) enantiomer samples ranged from 92 to 100. The test solution was
observed to be stable up to 24 h after the preparation. The developed method was also checked by different analysts and on
different lots of columns, reagents and it was proved to be rugged. The developed normal phase chiral LC method can be used
for the determination of the enantiomeric purity of R-β-amino-β-(4-methoxyphenyl) propionic acid. 相似文献
5.
G. Yu. Ishmuratov G. R. Mingaleeva O. O. Shakhanova R. R. Muslukhov M. P. Yakovleva L. P. Botsman A. G. Tolstikov 《Chemistry of Natural Compounds》2011,47(2):210-214
Optically active symmetric macrocyclic diesterazines and diesterdihydrazides were synthesized efficiently from the available
natural monoterpene (+)-α-pinene (de 50%) using a [2+1]-reaction of 1′-[(1S,3S)-3-(2hydroxyethyl)-2,2-dimethylcyclobutyl]ethanone
and glutaric and adipic acid chlorides followed by [1+1]condensation of the intermediate diketodiesters with hydrazine hydrate
or glutaric acid dihydrazide. 相似文献
6.
G. V. Grishina I. S. Veselov V. A. Davankov M. M. Il’in N. S. Zefirov 《Russian Journal of Organic Chemistry》2008,44(2):282-287
Enantiomeric pure (−)-(3R,4S)-1-benzyl-3,4-epoxypiperidine and (−)-(R)-1-benzyl-3-hydroxy-1,2,3,6-tetrahydropyridine with enantiomeric excess 61.9% were obtained by kinetic separation of (±)-1-benzyl-3,4-epoxypiperidine
under the action of lithium salt (+)-(S)-2-[(pyrrolidin-1-yl)methyl]pyrrolidine. The sterical direction of the kinetic separation of (±)-1-benzyl-3,4-epoxypiperidine
and absolute configurations of the target products were established.
Original Russian Text ? G.V. Grishina, I.S. Veselov, V.A. Davankov, M.M. Il’in, N.S. Zefirov, 2008, published in Zhurnal Organicheskoi
Khimii, 2008, Vol. 44, No. 2, pp. 287–291. 相似文献
7.
Nguyen Dam Phuc Le Y Kieu Thai Nhung Thi Tuyet Nguyen Tuan Trong Pham Nhat Vu Le Phuoc Huu Nguyen Tram Thi Thu 《Chemistry of Natural Compounds》2022,58(3):459-463
Chemistry of Natural Compounds - One new calamenene sesquiterpene glycoside, (1R,2R,3S,4S)-4-isopropyl-1,6-dimethyl-1,2,3,4- tetrahydronaphthalene-2,7-diol 3-O-β-D-glucopyranoside (1), along... 相似文献
8.
In order to provide insight into the reaction pathways of nitrogen oxide redox species with [Fe-S] models that may parallel those existing in biology, the reactivity of the iron-sulfur species, {[Fe(II)(S(4)NEt(2)N)]}(2) (1) and [Fe(II)(CH(3)CN)(S(4)NEt(2)N)] (2), where (S(4)NEt(2)N)(2-) = 2,6-bis(2-mercaptophenylthiomethyl)-4-diethylaminopyridine(2-), towards NO(+) (nitrosation) has been studied mechanistically in acetonitrile and compared with the corresponding reactions with NO (nitrosylation). For the nitrosation of 1, the reaction takes place in two steps that correspond to the nitrosation of the mononuclear (2) and dinuclear (1) complexes, respectively. For the corresponding carbonyl complex [Fe(II)(CO)(S(4)NEt(2)N)] (3), the nitrosation reaction occurs in a single step. The relative reactivity of the iron-sulfur species is approximately (1)/(2)/(3) = 1/20/10. Activation parameters for the nitrosation of 1 (ΔH(#) = 27 ± 1 kJ mol(-1), ΔS(#) = -111 ± 2 J K(-1) mol(-1), and ΔV(#) = -19 ± 2 cm(3) mol(-1)), 2 (ΔH(#) = 46 ± 2 kJ mol(-1), ΔS(#) = -22 ± 7 J K(-1) mol(-1), and ΔV(#) = -9.7 ± 0.4 cm(3) mol(-1)) and 3 (ΔH(#) = 38 ± 1 kJ mol(-1), ΔS(#) = -44 ± 4 J K(-1) mol(-1), and ΔV(#) = -7.8 ± 0.3 cm(3) mol(-1)) were determined from variable temperature and pressure studies. The significantly negative ΔS(#) and ΔV(#) values found for the nitrosation reactions are consistent with an associative mechanism. A comparative study of the reactivity of the iron-sulfur species 1 to 3 towards NO(+) and NO is presented. 相似文献
9.
N. E. Golantsov A. V. Karchava Z. A. Starikova F. M. Dolgushin M. A. Yurovskaya 《Chemistry of Heterocyclic Compounds》2005,41(10):1290-1299
A simple method is proposed for the synthesis of optically active indole-2-carbaldehydes via alkylation of 2-cyanoindole by
optically active secondary alcohols and subsequent reduction of the cyano group to an aldehyde. Reaction of the aldehydes
obtained with aromatic amines gave imines whose reaction with the Danishefsky diene was studied. The structure of the major
diastereomer of (2R′)-1-phenyl-2-[1-((1R′)-1-phenylethyl)indol-2-yl]-1,2,3,4-tetrahydropyridine-4-one and minor diastereomer
(2S)-2-[1-((1S)-2-methoxy-1-phenylethyl)indol-2-yl]-1-phenyl-1,2,3,4-tetrahydropyridine-4-one respectively were established
by X-ray analysis.
__________
Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1540–1550, October, 2005. 相似文献
10.
M. Madesclaire P. Coudert V. Gaumet V. P. Zaitsev Yu. V. Zaitseva 《Chemistry of Heterocyclic Compounds》2006,42(5):665-670
We have synthesized a series of (1R,2R,4S,5S,8S)-2,8-diaryl-4-(4-nitrophenyl)-1-aza-3,7-dioxabicyclo[3.3.0]octanes as a result
of reaction of (1S,2S)-2-amino-1-(4-nitrophenyl)-1,3-propanediol with aromatic aldehydes. The structure of the compounds obtained
was established on the basis of 1H NMR data.
__________
Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 5, pp. 757–763, May, 2006. 相似文献
11.
选取溴代噻唑和三乙炔基苯为单体,利用聚合反应自下而上构建含噻唑共轭微孔聚合物(NSCMP),通过热解和KOH活化热解NSCMP制备了氮、硫杂原子硬炭(NSHC)和活化NSHC(KNSHC)。利用扫描电子显微镜、能量色散谱、氮气吸附-脱附和恒流充放电等表征2个样品的结构与电化学性能。研究表明KNSHC中N和S的质量分数分别为10.42%和2.23%,KNSHC比表面积高达2 140 m2·g-1。在0.2 A·g-1电流密度下循环500次后KNSHC和NSHC的可逆比容量分别为946.2和493.7 mAh·g-1。KNSHC的优异电化学性能归因于其独特的孔结构和氮、硫杂原子的协同作用。 相似文献
12.
S. I. Orysyk L. N. Rybachuk V. I. Pekhnyo V. V. Orysyk 《Russian Journal of Inorganic Chemistry》2011,56(11):1747-1751
New Pd(II) complexes with 1-allyl-3-(2-pyridyl)thiourea (APTU) of the formulas [Pd(C9H11N3S)Cl2] (I) and [Pd(C9H11N3S)2]Cl2 (II) were obtained and examined by UV-Vis, IR, and 1H NMR spectroscopy. The conditions for the complexation reactions were optimized.
The instability constants and molar absorption coefficients of these complexes were calculated. Comparison of the characteristic
bands in the UV-Vis and IR spectra of the complexes and free APTU revealed that the ligand in both complexes is coordinated
to the metal atom in the thione form in the bidentate chelating mode through the S atom of the thiourea group and the pyridine
N atom. In the UV-Vis spectra of the complexes, the charge transfer bands (π → π* Py) and n → π* (C=NPy), (C=S) experience hypsochromic shifts by 450–470 cm−1 caused by the coordination of APTU to the metal ion, which gives rise to ligand-metal charge-transfer bands (C=NPy → Pd, n → π* (C=S)) and (SPd). The protons in the 6-, 4-, and 3-positions of the pyridine ring and the thiourea NH proton in the
chelate ring are most sensitive to the complexation. 相似文献
13.
A. R. Kudinov V. I. Meshcheryakov P. V. Petrovskii M. I. Rybinskaya 《Russian Chemical Bulletin》1999,48(1):176-178
Compounds (η-C5R5)Fe[η-9-(Me2S)-7,8-C2B9H10] (R=H, Me) and (η-C4Me4)Co[η-9-(Me2S)-7,8-C2B9H10] were synthesized by the reactions of Na[9-(Me2S)-7,8-C2B9H10] with complexes [(η-C5H5)Fe(MeCN)3]PF6, [(η-C5Me5)Fe(MeCN)3]BF4, and [(η-C4Me4)Co(MeCN)3]PF6, respectively.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 1, pp. 177–179, January, 1999. 相似文献
14.
M. Madesclaire P. Coudert V. P. Zaitsev J. V. Zaitseva 《Chemistry of Heterocyclic Compounds》2006,42(4):506-511
A series of isomeric 2-oxazolidinones has been synthesized from (1S, 2S)-2-amino-1-(4-nitrophenyl)-1,3-propanediol.
__________
Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 4, pp. 579–584, April, 2006. 相似文献
15.
G. V. Shevchuk Yu. S. Vollerner A. S. Shashkov M. B. Gorovits V. Ya. Chirva 《Chemistry of Natural Compounds》1991,27(6):706-711
Two new glycosides which have been called nolinofurosides G(I) and H(III), have been isolated from the leaves ofNolina microcarpa. Nolinofuroside G is the sodium salt of 26-β-D-glucofuranosyloxy-(25S)-furost-5,20(22)-diene-1β, 3β-diol 1-sulfate, and nolinofuroside
H is the sodium salt of 1-β-D-fucopyranosyloxy-26-β-D-glucopyranosyloxy-(25S)-furost-5,20(22)-dinen-1β-3β-ol 3-sulfate.
M. V. Frunze Simferopol' State University. Institute of the Chemistry of Plant Substances, Uzbek. Academy of Sciences, Tashkent.
Translated from Khimiya Prirodnykh Soedinenii, No. 6, pp. 801–806, November–December, 1991. 相似文献
16.
Planar chiral 2- and 3-bicymantrenylcarbaldehydes can be resolved to enantiomers through Schiff's bases with (S)-(−)-α-phenylethylamine.
Optically active derivatives of bicymantrenyl with Me and CH2OH substituents were synthesized from (−)-3-bicymantrenylcarbaldehyde. The absolute configuration of Schiff's base obtained
from (+)-3-bicymantrenylcarbaldehyde was determined by X-ray diffraction analysis.
For Part 3, see Ref. 1.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 1, pp. 158–162, January, 1997. 相似文献
17.
V. R. Akhmetova E. B. Rakhimova A. B. Minnebaev R. V. Kunakova N. F. Galimzyanova 《Russian Journal of Organic Chemistry》2012,48(2):202-208
Cyclothiomethylation was performed of heterochain (O, S-S, NH) α,ω-diamines with formaldehyde and H2S in aqueous medium at 20–60°C to obtain new α,ω-bis(1,3,5-dithiazinanes). The cyclocondensation of N-(3-aminopropyl)butane-1,4-diamine
(spermidine), formaldehyde, and H2S proceeds efficiently in the medium of BuOH-H2O at 0°C and leads to the formation of previously unknown O,S-containing macroheterocycle, 1,7-dioxa-3,5,9,11-tetrathiacyclododecane.
A fungicidal activity was found in 5,5′-(3,6-dioxaoctane-1,8-diyl)bis-1,3,5-dithiazinane with respect to microscopic fungi
affecting agriculture. 相似文献
18.
19.
Chiral bridge-substituted manganese(III) complexes of N,N′-bis-(2-hydroxynaphthalene-1-carbaldehyde)-(1R,2R)-(−)-diaminocyclohexane and N,N′-bis-(2-hydroxynaphthalene-1-carbaldehyde)-(1S,2S)-(+)-diaminocyclohexane have been synthesized. The interaction of these
complexes with calf thymus DNA(CT-DNA) was investigated by spectroscopic, thermal denaturation studies, circular dichroism
(CD), and viscosity measurements. Results of spectroscopic and viscosity measurements suggest that the two complexes bind
to DNA via an intercalative mode and display enantioselectivity. These Mn(III) complexes have been found to promote the cleavage
of plasmid DNA pBR322 in the presence of H2O2. 相似文献
20.
Silvia M. C. S. Monteiro Armando J. D. Silvestre Artur M. S. Silva José A. S. Cavaleiro 《Monatshefte für Chemie / Chemical Monthly》2008,139(9):1119-1126
The synthesis of new flavone-type compounds bearing several chiral centres, 12- and 14-(2′-chromonyl)dehydroabietates, are
reported. This synthesis started from the aldol condensation of methyl 12- and 14-formyldehydroabietates with 2′-hydroxyacetophenones
in order to prepare the corresponding chalcone-type compounds, which were then transformed in the expected flavone-type compounds
by cyclodehydrogenation with DMSO and a catalytic amount of iodine. All compounds were exhaustively characterised by NMR and MS techniques.
Present address: Silvia M. C. S. Monteiro, Environment Department, Polytechnic Institute of Leiria, 2411–901 Leiria, Portugal.
Correspondence: José A. S. Cavaleiro, Chemistry Department, University of Aveiro, 3810-193 Aveiro, Portugal. 相似文献