共查询到20条相似文献,搜索用时 22 毫秒
1.
N. Yu. Kuznetsov K. A. Lyssenko A. S. Peregudov Yu. N. Bubnov 《Russian Chemical Bulletin》2007,56(8):1569-1574
A method for the synthesis of bridged azabicyclic compounds from isoquinolines was developed. The method is based on a combination
of allylboration and ruthenium-catalyzed intramolecular metathesis. Reductive 1,3-diallylation of bromoisoquinolines with
triallylborane gave trans-1,3-diallyl-1,2,3,4-tetrahydroisoquinolines. When heated with triallylborane, these compounds yielded mixtures of cis-and trans-isomers in the ratio ∼1: 1. The structure of cis-1,3-diallyl-5-bromo-1,2,3,4-tetrahydroisoquinoline was confirmed by X-ray diffraction analysis. In a similar way, trans-3-allyl-1-vinyl-1,2,3,4-tetrahydroisoquinoline synthesized by sequential vinylation (with vinyllithium) and allylboration
of isoquinoline, yielded a mixture of cis-and trans-isomers in the ratio 1.6: 1. Intramolecular metathesis reactions of N-Boc derivatives of cis-isomers in the presence of the Grubbs catalyst (2.0–2.5 mol.%) afforded 7,8-benzo-10-azabicyclo[4.3.1]dec-2-enes or 7,8-benzo-9-azabicyclo[3.3.1]non-2-ene
in nearly quantitative yields.
Dedicated to Academician V. A. Tartakovsky on the occasion of his 75th birthday.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 1510–1515, August, 2007. 相似文献
2.
D. L. Lipilin A. Yu. Tyurin O. Yu. Smirnov A. M. Churakov Yu. A. Strelenko V. A. Tartakovsky 《Russian Chemical Bulletin》2006,55(7):1239-1242
Treatment of 2-(tert-butyl)-1,2,3,4-benzotetrazinium tetrafluoroborates with sodium thiocyanate afforded 2-(tert-butylazo)phenyl isothiocyanates 3, which exist in equilibrium with 2-(tert-butyl)-1,2,4-benzotriazine-3(2H)-thiones 3′. The equilibrium depends on the substituents R in the benzene ring: the percentage of the open isomer 3 is about 20% for R = H or Me; for R = Cl or Br, the equilibrium is completely shifted to cyclic isomer 3′. The equilibrium is slow on the time scale of the 1H and 13C NMR experiments. For compounds 3a/3′a (R = H), the spectra at 24 °C show two sets of signals, while those at 0 °C contain only signals for isomer 3′a.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 7, pp. 1192–1195, July, 2006. 相似文献
3.
K. F. Koehler H. Zaddach A. D. Kuntsevich V. N. Voznesenskii I. I. Chervin R. G. Kostyanovsky 《Russian Chemical Bulletin》1993,42(10):1757-1759
The1H and13C NMR spectral parameters of α-, β-, and y-lewisites1–5 were obtained and a new isomer,cis,trans,trans-γ-lewisite5, was isolated and identified on the basis of chemical shifts, relative intensities of the signals, and the intra-chain (3
J
hh
,3
J
ch
) and interchain (3
J
casch
) coupling constants.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 10, pp. 1833–1835, October, 1993. 相似文献
4.
Apyari VV Dmitrienko SG Ostrovskaya VM Anaev EK Zolotov YA 《Analytical and bioanalytical chemistry》2008,391(5):1977-1982
Polyurethane foam (PUF) has been suggested as a solid polymeric reagent for determination of nitrite. The determination is
based on the diazotization of end toluidine groups of PUF with nitrite in acidic medium followed by coupling of polymeric
diazonium cation with 3-hydroxy-7,8-benzo-1,2,3,4-tetrahydroquinoline. The intensely colored polymeric azodye formed in this
reaction can be used as a convenient analytic form for the determination of nitrite by diffuse reflectance spectroscopy (c
min = 0.7 ng mL−1). The possibility of using a desktop scanner, digital camera, and computer data processing for the numerical evaluation of
the color intensity of the polymeric azodye has been investigated. A scanner and digital camera can be used for determination
of nitrite with the same sensitivity and reproducibility as with diffuse reflectance spectroscopy. The approach developed
was applied for determination of nitrite in river water and human exhaled breath condensate. 相似文献
5.
V. P. Rybalkin E. N. Shepelenko V. V. Tkachev G. V. Shilov S. K. Balenko A. V. Tsukanov L. L. Popova A. D. Dubonosov S. M. Aldoshin V. A. Bren’ V. I. Minkin 《Russian Chemical Bulletin》2006,55(1):101-105
New photochromic fulgide, viz., 4-{1-[2-(anthracen-9-yl)-5-methyloxazol-4-yl]ethylidene}-3-isopropylidenetetrahydrofuran-2,5-dione, with fluorescent properties
was synthesized. Studies by electronic, IR, and 1H NMR spectroscopy and X-ray diffraction demonstrated that this fulgide exists in the Z form. Light irradiation of its solutions at a wavelength of 365 nm causes Z/E isomerization giving rise to the thermally stable cyclic form. The latter is transformed into the starting E isomer under light irradiation at λ = 436 nm.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 1, pp. 97–101, January, 2006. 相似文献
6.
Sumera Mahboob Rohama Gill Muhammad Mazhar Gabriele Kociok-Köhn Kieran C. Molloy 《Monatshefte für Chemie / Chemical Monthly》2008,139(9):1019-1024
A series of trichlorogermyl-substituted dicarboxylic acids of general formula HOOC–R′–COOH where R′=–CH2CH(GeCl3)CH2– 1, –CH(CH2GeCl3)CH2– 2, –CH(GeCl3)CH2– 3 and –CH(CH3)CH(GeCl3)– 4 were synthesized by the hydrogermylation reaction of unsaturated acids, such as trans-glutaconic (2-pentenedioic acid), itaconic (methylenebutanedioic acid), fumaric (2-butenedioic acid), and citraconic (2-methyl-2-butenedioic
acid) acids with HGeCl3, which was produced in situ by the reaction of GeO2 with 37% HCl in presence of NaH2PO2 · H2O. All these compounds were characterized by melting point, CHN analysis, FTIR, and multinuclear NMR (1H; 13C; H,H-COSY). X-Ray crystal structures of 1 and 2 were analyzed to show supramolecular structures in which central Ge atom in each of these structures is four-coordinated
with a slightly distorted tetrahedral geometry. Structurally, both compounds adopt supramolecular forms via strong intermolecular O–H–O interactions through 8-membered and 22-membered hydrogen bonded rings.
Supplementary material to this paper is available in electronic form at
Correspondence: Muhammad Mazhar, Department of Chemistry, Quaid-i-Azam University, Islamabad 45320, Pakistan. 相似文献
7.
V. R. Khairullina A. Ya. Gerchikov G. G. Garifullina Ya. B. Drevko O. V. Fedotova 《Kinetics and Catalysis》2010,51(1):38-41
The antioxidant properties of 2,4-diphenyl-7,8-benzo-5,6-dihydro(4H)selenochromene and 2-para-chlorophenyl-4-phenyl-7,8-benzo-5,6-dihydro(4H)selenochromene were studied using the initiated oxidation of ethylbenzene
and propan-2-ol as model reactions. The antioxidant activity of these compounds was quantitatively characterized by the apparent
rate constant of inhibition, fk
in. Addition of 2,4-diphenyl-7,8-benzo-5,6-dihydro(4H)selenochromene to ethylbenzene being oxidized increases the chemiluminescence
intensity. 相似文献
8.
D. A. Rudakov V. I. Potkin E. A. Dikusar P. V. Petrovskii I. B. Sivaev V. I. Bregadze 《Russian Chemical Bulletin》2007,56(5):922-925
Treatment of potassium 7,8-dimethyldecahydro-7,8-dicarba-nido-undecaborate with N-chloro-and N-bromosuccinimides in acetonitrile or with an excess of iodine in methanol gave the corresponding dihalo derivatives [9,11-X2-7,8-Me2-7,8-C2B9H8]− (X = Cl, Br, or I), which were isolated as alkylammonium salts. The compound (Me3NH)+[9,11-I2-7-Me-7,8-C2B9H9]− was synthesized by a reaction of K+[7-Me-7,8-C2B9H11]− with an excess of iodine in methanol. The compounds obtained were characterized by IR and NMR (1H, 11B, and 11B-11B COSY) spectroscopy.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 5, pp. 888–891, May, 2007. 相似文献
9.
D.I. Kim E.H. Kim T.G. Roy Z.U. Bae J.H. Choi H.G. Na Y.C. Park 《Journal of inclusion phenomena and macrocyclic chemistry》2005,53(3):211-217
13,14-Benzo-5,8-dihydro-2,4,9,11-tetramethyl-1,5,8,12-tetraazacyclotetradeca-1,3,9,11-tetraene and 13,14-benzo-3,10-di(p-[X]benzoyl)-5,8-dihydro-2,4,9,11-tetramethyl-1,5,8,12-tetraazacyclotetradeca-1,3,9,11-tetraene, wherein X = CH3, H, Cl, NO2 and OCH3, were synthesized and characterized. IR spectra of the benzoylated compounds showed an intense band assigned to the stretching modes of C==O in the region 1632 ~ 1638 cm−1. Hammett plot of the energies of π → π* for the compounds was linear with a positive slope (+0.923). 1H NMR signals exhibited a deshielding effect due to benzoyl groups, while methyl protons only exhibited the shielding effect by the magnetic anisotropy of the group. The substituent effect on 13C NMR was similar to that on proton NMR. The cyclic voltammograms of the compounds mostly showed two one-electron irreversible oxidation peaks and one or two reduction waves between −0.280 and −2.500 V depending on the substituents. Hammett plots of 1st and 2nd oxidation potentials (Eop(1) and Eop(2)) were linear with slopes of +0.036 and +0.045, respectively. The structure of the compound 4 (monoclinic, C2/c, a = 26.0059 (19), b = 6.9058 (5), c = 33.082 (2), β = 109.5930°, Z = 8) was determined using X-ray diffraction method. 相似文献
10.
A. V. Okotrub L. G. Bulusheva G. G. Furin V. V. Murakhtanov 《Russian Chemical Bulletin》1998,47(12):2362-2370
The high resolution X-ray emission O-Kα spectra of pentafluorophenylalkyl ethers C6F5OR (R=Et, Pri, and But) exhibit differences related to a change in the electronic structure of the compounds as R is varied. The search for stable
conformers was performed by the semiempirical PM3 method. The most probable structures of C6F5OR were determined by the comparison of the experimental and theoretical X-ray spectra plotted for each conformer usingab initio calculations in the 6–31 G basis set. Substituent R in pentafluorophenylalkyl ethers is situated outside of the ring plane.
The fluorination of the benzene ring changes the energy level of the lone electron pair of oxygen relative to the levels of
orbitals of the ring and substituent R and leads to an increase in the efficiency of interactions in the σ-system.
Deceased.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 12, pp. 2443–2450, December, 1998. 相似文献
11.
Reaction of [Ni(dppe)Cl2/Br2] with AgOTf in CH2Cl2 medium following ligand addition leads to [Ni(dppe)(OSO2CF3)2] and then [Ni(dppe)(RaaiR)](OSO2CF3)2 [RaaiR′ = p–R–C6H4–N=N–C3H2–NN-1–R′,(1–3), abbreviated as N,N′-chelator, where N(imidazole) and N(azo) represent N and N′, respectively; R = H (a), Me (b), Cl (c) and R′ = Me (1), CH2CH3
(2), CH2Ph (3), OSO2CF3 is the triflate anion]. 31P{1H}-NMR confirm that stable bis-chelated square planar Ni(II) azoimine–dppe complex formation with one sharp peaks. The 1H NMR spectral measurements suggest azoimine link is present with lot of phenyl protons in the aromatic region. Considering
all the moities there are a lot of different carbon atoms in the molecule which gives many different peaks in the 13C(1H)-NMR spectrum. In the 1H-1H COSY spectrum in the present complexes and contour peaks in the 1H-13C-HMQC spectrum in the present complexes, assign the solution structure and stereoretentive conformation in each complexes. 相似文献
12.
V. M. Ostrovskaya A. V. Tsygankov O. A. Prokopenko A. K. Buryak E. A. Reshetnyak N. A. Nikitina 《Journal of Analytical Chemistry》2008,63(8):792-798
RIB-Nitrite-Test and Sorbfil-Nitrite-Test strips were developed for determining nitrite ions in water samples and foodstuffs by a reaction similar to the Griess reaction. Stable and noncarcinogenic 3-hydroxy-7,8-benzo-1,2,3,4-tetrahydroquinoline was used as an azo component adsorbed in the reagent paper zone on a polymeric support or on a Sorbfil plate sealed in a transparent polymeric film. Performance characteristics were evaluated by a statistical method for visual test procedures for the detection and determination of NO 2 ? using two different test strips. The determination limit was 0.54 and 0.09 mg/L, and the detection limit was 0.50 and 0.08 mg/L, respectively. 相似文献
13.
Reaction of [Au2(dppm)Cl2] with AgOTf in CH2Cl2 medium followed ligand addition and leads to [Au2(dppm)(RaaiR′)](OTf) [RaaiR′ = p-R–C6H4–N = N–C3H2–NN–1–R′, (1–3), abbreviated as N,N′-chelator, where N(imidazole) and N(azo) represent N and N′, respectively; R = H (a), Me (b), Cl (c) and R′ = Me (1), CH2CH3
(2), CH2Ph (3), OSO2CF3 is the triflate anion, and dppm is the diphenylphosphinomethane-ring]. The 1H-n.m.r. spectral measurements suggest methylene, –CH2–, in RaaiEt gives a complex AB type multiplet while in RaaiCH2Ph it shows AB type quartets with coupling constant of avg. 6 Hz. Considering all the moities there are a lot of different
carbon atoms in the molecule which gives a lot of different peaks in the 13C-n.m.r spectrum. In the 1H–1H-COSY spectrum of the present complexes and contour peaks in the 1H–13C-HMQC spectrum in the present complexes, assign the solution structure and stereoretentive transformation in each step. 相似文献
14.
Harald Stueger Markus Braunwarth Gottfried Fuerpass Judith Baumgartner Robert Saf 《Monatshefte für Chemie / Chemical Monthly》2006,137(5):595-603
Summary. The previously unknown ruthenio disilanes Rp–Si2Me4–C6H4X (Rp = η5-C5H5Ru(CO)2; X = H, Br, –CHO, CH=C(CN)2) were synthesized from ClSi2Me4C6H4X (X = H, Br) and Rp− using conventional chemical methods. Trends in the UV/Vis absorption spectra indicate strong electronic coupling within the
Rp–Si–Si–Caryl fragment and, therefore, closely resemble the ones observed for the corresponding iron complexes. The four compounds however,
were shown to be less sensitive towards UV irradiation. The crystal structure of Rp–Si2Me4–C6H4CH=C(CN)2 was determined by X-ray diffraction and exhibits an all-trans-array of the Ru–Si–Si–Caryl moiety, what is a basic requirement for optimal through-bond interaction. 相似文献
15.
Prithwiraj Byabartta 《Transition Metal Chemistry》2007,32(3):304-313
Reaction of [Au(PPh3)2(tht)2](OSO2CF3)3 with RaaiR′ in CH2Cl2 medium following ligand addition leads to [Au(PPh3)2(RaaiR′)](OTf)3 [RaaiR′ = p-R–C6H4–N=N–C3H2–NN–1–R′, (1–3), abbreviated as N,N′-chelator, where N(imidazole) and N(azo) represent N and N′, respectively; R = H (a), Me (b), Cl (c) and R′ = Me (1), CH2CH3
(2), CH2Ph (3), PPh3 is triphenylphosphine, OSO2CF3 is the triflate anion, tht is tetrahydrothiophen]. The maximum molecular peak of the corresponding molecule is observed in
the ESI mass spectrum. The 1H-nmr spectral measurements suggest methylene, –CH2–, in RaaiEt gives a complex AB type multiplet while in RaaiCH2Ph it shows AB type quartets. 13C-nmr spectrum suggests the molecular skeleton. In the 1H–1H COSY spectrum as well as contour peaks in the 1H–13C heteronuclear multiple-quantum coherence (HMQC) spectrum assign the solution structure. Electrochemistry assign ligand reduction
part rather than metal oxidation. 相似文献
16.
D. P. Krut'ko M. V. Borzov E. N. Veksler E. M. Myshakin D. A. Lemenovskii 《Russian Chemical Bulletin》1998,47(5):956-959
Treatment of a mixture of isomeric (2-chloroethyl)-1,2,3,4-tetramethylcyclopentadienes with lithium diphenylphosphide leads
to novel 4,5,6,7-tetramethylspiro[2,4]hepta-4,6-diene among the reaction products. The reaction of spiroheptadiene obtained
with excess LiPPh2 at elevated temperature affords lithium 5-(2-diphenylphosphinoethyl)-1,2,3,4-tetramethylcyclopentadienide in almost quantitative
yield. the regioselectivity of alkylation of the tetramethylcyclopentadienide anion is estimated from quantum-chemical calculations
performedab initio for C5Mc4H−. The full charges on the ring carbon atoms are determined within the framework of Bader's theory of atomic fragments in molecules.
Translated fromIzvestiya Akademii Nauk. Seriya, Khimicheskaya, No. 5, pp. 986–989, may, 1998. 相似文献
17.
Yakunina I. E. Shakhkeldyan I. V. Atroshenko Yu. M. Borbulevich O. Ya. Nesterov V. V. Kopyshev M. B. Troitskii N. A. Efremov Yu. A. Alifanova E. N. Subbotin V. A. 《Russian Journal of Organic Chemistry》2004,40(2):239-246
A number of 3-R-9-(2-oxopropyl)-1,5-dinitro-7,8-benzo-3-azsbicyclo[3.3.1]non-7-en-6-ones was synthesized by Mannich reaction involving Yanovsky adduct of 2,4-dinitronaphthol. It was established by molecular spectroscopy and X-ray diffraction analysis that the piperidine ring in these compounds was in the chairconformation with a diequatorial position of the substituent attached to the heteroatom and 2-oxo-propyl group, and the cyclohexenone fragment was in sofaform. By an example of 3-methyl-9-(2-oxopropyl)-1,5-dinitro-7,8-benzo-3-azsbicyclo[3.3.1]non-7-en-6-one the dissociative ionization of bicyclononanes under the electron impact was investigated. 相似文献
18.
Raghavendra Kumar P. Ajai K. Singh J. E. Drake M. B. Hursthouse M. E. Little 《Structural chemistry》2007,18(2):203-207
A non-Schiff base (Te, N, O) ligand MeOC6 H4TeCH2CH2NHCH(CH3)C6H4–2–OH (LH) having a chiral center and its palladium(II) complex [PdClL]·CH2Cl2 (1) have been synthesized. Both have characteristic 1H and 13C NMR spectra. The single crystal structure of the complex 1 has been determined by X-ray diffraction methods. The monoclinic crystals of 1 (space group P21/n) have a=14.581(5) Å, b=13.160(5) Å and c=20.249(5) Å, β=99.398(5)°. The Te $\cdots A non-Schiff base (Te, N, O) ligand MeOC6 H4TeCH2CH2NHCH(CH3)C6H4–2–OH (LH) having a chiral center and its palladium(II) complex [PdClL]·CH2Cl2 (1) have been synthesized. Both have characteristic 1H and 13C NMR spectra. The single crystal structure of the complex 1 has been determined by X-ray diffraction methods. The monoclinic crystals of 1 (space group P21/n) have a=14.581(5) ?, b=13.160(5) ? and c=20.249(5) ?, β=99.398(5)°. The TeCl secondary interactions [3.303(2)–3.352(2) ?] between two nearly square planar palladium complex molecules results in a
bimolecular aggregate having a PdPd distance 3.203(1) ?. The Pd–Te, Pd–N and Pd–O bond lengths are 2.5005(7)/2.4914(7), 2.060(4)/2.061(4) and 2.054(3)/2.044(3) ?,
respectively. 相似文献
19.
Prithwiraj Byabartta 《Transition Metal Chemistry》2005,30(7):804-813
Ag+ assisted aquation of blue cis-trans-cis-RuCl2(RaaiR′)2 (4–6) leads to the synthesis of solvento species, blue-violet cis-trans-cis-[Ru(OH2)2(RaaiR′)2](ClO4)2 [Raai R′=p-R-C6H4
N=N–C3H2–NN–1–R′, (1–3), abbreviated as N,N′-chelator, where N(imidazole) and N(azo) represent N and N′, respectively; R = H (a), OMe (b), NO2 (c) and R′ = Me (1/4/7/10), CH2CH3 (2/5/8/11), CH2Ph (3/6/9/12)] that have been reacted with NO2−in warm EtOH resulting in violet dinitro complexes of the type, Ru(NO2)2(RaaiR′)2 (7–9). The nitrite complexes are useful synthons of electrophilic nitrosyls, and on triturating the compounds, (7b–9b) with conc. HClO4 nitro-nitrosyl derivatives, [Ru(NO2)(NO)(OMeaaiR′)2](ClO4)2 (10b–12b) are isolated. The solution structure and stereoretentive transformation in each step have been established from 1H n.m.r. results. All the complexes exhibit strong MLCT transitions in the visible region. They are redox active and display
one metal-centred oxidation and successive ligand-based reductions. The redox potentials of Ru(III)/Ru(II) (E1/2M) of (10b–12b) are anodically shifted by ∼
∼0.2 V as compared to those of dinitro precursors, (7b–9b). The ν(NO) >1900 cm−1 strongly suggests the presence of linear Ru–NO bonding. The electrophilic behaviour of metal bound nitrosyl has been proved
in one case (12b) by reacting with a bicyclic ketone, camphor, containing an active methylene group and an arylhydrazone with an active methine
group, and the heteroleptic tris chelates thus formed have been characterised. 相似文献
20.
A. R. Shaikhlislamova N. A. Zhuravlev A. B. Yaroslavtsev 《Russian Journal of Inorganic Chemistry》2010,55(1):18-22
H3 − 2x
Nb
x
M2 − x
(PO4)3 (M = In, Fe) acid phosphates have been obtained by ion exchange from their lithium forms and X-ray powder diffraction, impedance
measurements, and 7Li and 1H NMR spectroscopy. The parameters of the hexagonal unit cell of the proton-exchanged forms differ only slightly from those
of the initial lithium compounds. According to 1H NMR data, the proton in the acid phosphates is not hydrated. The conductivity of the acid phosphates at high temperatures
depends weakly on their composition and is ∼1.7 × 10−7 S cm−1 at 620 K. The activation energy of conduction is 30–33 kJ/mol (430–770 K). 相似文献