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1.
Lilija I. Kasyan Sergey V. Sereda Konstantin A. Potekhin Andrey O. Kasyan 《Heteroatom Chemistry》1997,8(2):177-184
A number of N-(arylsulfonyl)bicyclo[2.2.1]hept-2-enendo-5-methylamines have been synthesized from bicyclo[2.2.1]hept-2-en-endo-5-carbonitrile via reduction of the latter by lithium aluminum hydride and subsequent reactions of the resulting amine with arylsufonyl chlorides. The structures and stereochemical homogeneity of the products have been supported by the analysis of 1H NMR spectra and by COSY-experiments. The reactions of the sulfonamides with peroxyphthalic acid are accompanied by intramolecular cyclizations and are completed by the formation of N-(arylsulfonyl)-exo-2-hydroxy-4-azatricyclo[4.2.1.03,7]nonanes. The structures of the substituted azabrendanes have been confirmed by spectral methods. The molecular structure of N-(p-methoxy-carbonylaminophenylsulfonyl)-exo-2-hydroxy-4-azatricyclo-[4.2.1.03,7]nonane 8j has been determined by X-ray diffraction analysis. © 1997 John Wiley & Sons, Inc. 相似文献
2.
Threonine Schiff base derived 2-hydroxy-1-naphthaldehyde and threonine has been isolated and investigated. The stoichiometry of this compound was derived from the results of elemental analyses, IR, 1H-NMR and UV spectroscopic techniques. X-ray diffraction method was also used to obtain the single-crystal structure. The compound crystallizes in the space group P21 with cell dimensions a=5.109(2), b=11.334(2), and β=91(3)° with Z=2. The molecule has phenol-imine tautomeric form in the crystal structure. Some of bond lengths and angles found in the molecular structure are distorted due to π-electron delocalization and steric effect of naphthylidene and threonine groups. 相似文献
3.
Meriem Lamouchi Erwann JeanneauJérémy Coulm Arnaud BrioudeCédric Desroches 《Comptes Rendus Chimie》2013,16(12):1073-1078
A simple method for thiacalix[4]arene O-monoamide preparation with high yields using 5,11,17,23-tetra-tert-butyl-28-(ethoxycarbonyl)methoxy-2,8,14,20-tetrathiacalix[4]arene reaction with diaminoalkanes is reported. The solid state cyclization reaction of the acylethylenediamines function of 5,11,17,23-tetra-tert-butyl-28-O-[(N-(2-aminoethyl)aminocarbonyl)-methoxy]thiacalix[4]arene leading to the formation of the 5,11,17,23-tetra-tert-butyl-28-[2-methoxy-imdazoline]thiacalix[4]arene compound is described for the first time for the calixarene macrocycle family. Finally, preliminary results show that O-mono-amide-thiacalixarene derivatives are promising candidates for the production of self-assembled materials and efficient precursors for the synthesis of bisthiacalix[4] arenes. 相似文献
4.
Efficient routes for the synthesis of 4-azahomoadamantane (V) via the Beckmann and Schmidt rearrangements are described. The lactam III is unusual in that it forms a stable crystalline hydrochloride IV. 相似文献
5.
The reaction of boron heterocycles 1 and 2 with n-butyl lithium and alkyl halides led to (N→B) phenyl[N-alky-N-(2-alkyl)aminodiacetate-O,O′,N]boranes 3–6(a–b), 7(b) and 9(b), where alkyl can be in exo and/or endo position, and phenyl[N-alkyl-N-(2-alkyl)aminodiacetate-O,O′,N]boranes 7(c) and 8(c) isomers, which do not display the intramolecular N→B coordination bond. The existence of steric interactions between N-benzyl and the alkyl group at 2 position was indicated by 1H and 13C NMR, while, the δ(11B) values confirm the tetrahedral and trigonal environment of the 11B nucleus in these compounds. Moreover, the compounds were characterized by COSY, HETCOR and homonuclear proton decoupling experiment. The study of the intramolecular N→B coordination by dynamic NMR afforded a ΔG‡ value of 81.09 kJ/mol for compound 6(b). 相似文献
6.
《Tetrahedron》1987,43(2):377-381
An improved method for the synthesis of 4-azatricyclo [5.2.2.04,8] undecan-11-one (1) is reported. The synthesis involves hydrogenolysis of 8-hydroxyethyl-2-azabicyclo [3.3.1] nonan-7-one 3 followed by intramolecular alkylation of the resulting secondary amine 7. The required azabicyclic alcohol 3 was obtained by oxidative cyclization with mercuric acetate of the α-alkylated methyl 4-piperidineacetoacetate 5. 相似文献
7.
Yingzhong Shen Yan Wang Yiying Zhang Ye Li Xian Tao Huihua Xu 《Journal of organometallic chemistry》2007,692(24):5345-5350
Three dimethylgallium complexes of type Me2GaL [L = 2-methoxylphenylmethyleneiminophenolato (1), N-(4-N,N′-dimethylamino)phenylmethyleneiminophenolato (2), N-(2-naphthyl)methyleneiminophenolato (3)] have been synthesized by the reaction of trimethylgallium with appropriate N-arylmethyleneiminophenol. The complexes obtained have been characterized by elemental analysis, 1H, 13C{1H} NMR, IR and mass spectroscopy, respectively. The solid structure of 2 has been determined by X-ray single crystal analysis. The gallium atom was bonded by an oxygen atom and coordinated by an imine nitrogen atom forming one five-membered ring. The stable dimmer was formed by the coordination of bridging oxygen atom of phenolate to another gallium atom. The photoluminescence of complexes 1-3 were studied. The maximum emission wavelengths of 1-3 are between 305 and 320 nm upon radiation by UV light. The electroluminescent properties of diodes using 1-3 as emitting material were measured. The blue/green electroluminescence has been observed. 相似文献
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9.
Andrea Buzas Xavier F. Le Goff Fabien Gagosz 《Journal of organometallic chemistry》2009,694(4):515-10978
A study concerning the gold(I)-catalyzed transformation of N-(hex-5-enynyl) tert-butyloxycarbamates is described. The mild conditions employed allow the moderately efficient but stereoselective synthesis of a range of bicyclic carbamates following a formal [4+2] cycloaddition process. 相似文献
10.
A new dicarboxylic acid, N-[3,5-bis(N-trimellitoyl)phenyl]phthalimide (1a), bearing three preformed imide rings was synthesized from the condensation of N-(3,5-diaminophenyl)phthalimide and trimellitic anhydride in glacial acetic acid at 1:2 molar ratio. For study of structure-properties relationship 1,3-bis(N-trimellitoyl)benzene (1b, as a reference) was also synthesized in a similar manner. 1a and 1b were characterized by spectroscopic methods and elemental analyses.A series of wholly aromatic poly(amide-imide)s with inherent viscosities of 0.63-1.09 dl g−1 was prepared by triphenyl phosphite-activated polycondensation from the triimide-dicarboxylic acid 1a and the reference monomer 1b with various aromatic diamines. All of the polymers were fully characterized by FT-IR and 1H NMR spectroscopy. The effects of the phthalimide pendent group on the polymers properties such as solubility, crystallinity, and thermal stability were investigated by comparison of the polymers. The polymers obtained from triimide-dicarboxylic acid 1a exhibited excellent solubility in a variety of solvents such as N-methyl-2-pyrrolidone, N,N-dimethylacetamide, N,N-dimethylformamide, and dimethylsulfoxide. These poly(amide-imide)s possessed glass-transition temperatures from 334 to 403 °C and exhibited excellent thermal stabilities and had 10% weight losses from 541 to 568 °C under a nitrogen atmosphere. Poly(amide-imide)s containing phthalimide pendent groups showed higher solubility, higher Tg and Td10% values than those having no phthalimide pendent groups. 相似文献
11.
A convenient, high-yield synthesis of N-Boc-7-azabicyclo[2.2.1]hept-5-en-2-one (7) was developed by SmI2-mediated desulfonylation of 6. Thus, 5-endo-, 5-exo-, 6-endo-, and 6-exo-hydroxylated epibatidine analogues 2a,b and 3a,b were synthesized from 7 by using a Pd(PPh3)4-catalyzed reductive Heck coupling reaction and SmI2-mediated reduction of the carbonyl group as the key steps. Other reaction conditions for the reductive Heck procedure and the reduction step were also investigated. 相似文献
12.
Grafting of N,N-dimethyl-N-methacryloxyethyl-N-(3-sulfopropyl) ammonium (DMMSA) onto chitosan using ceric ammonium nitrate as an initiator was studied under nitrogen atmosphere in 2% wt. acetic acid solution. The grafted polymer was confirmed by FT-IR spectroscopy. The extent of grafting could be adjusted by controlling the appropriate reaction conditions. The maximum percentage of grafting about 50% was obtained under optimum condition. A representative grafted copolymer was characterized by thermogravimetric analysis and chitosan was used as reference. 相似文献
13.
Hossein Behniafar Batool Akhlaghinia Sedigheh Habibian 《European Polymer Journal》2005,41(5):1071-1078
A new dicarboxylic acid chloride (2) bearing three preformed imide rings was synthesized by treating N-(3,5-diaminophenyl)phthalimide with trimellitic anhydride followed by refluxing with thionyl chloride. A novel family of aromatic poly(ester-imide)s with inherent viscosities of 0.27-0.35 dl g−1 were prepared from 2 with various bisphenols such as resorcinol (3a), hydroquinone (3b), 2,2′-dihydroxybiphenyl (3c), 4,4′-dihydroxybiphenyl (3d), bisphenol-A (3e), 2,2′-dimethyl-4,4′-dihydroxybiphenyl (3f), 1,5-dihydroxynaphthalene (3g), 2,7-dihydroxynaphthalene (3h), and 2,2′-dihydroxy-1,1′-binaphthyl (3i) by high-temperature solution polycondensation in nitrobenzene using pyridine as hydrogen chloride quencher. All of the resulted polymers were fully characterized by FT-IR and NMR spectroscopy and elemental analyses. The poly(ester-imide)s exhibited excellent solubility in some polar organic solvents. From differential scanning calorimetry, the polymers showed glass-transition temperatures between 259 and 353 °C. Thermal behaviors of the obtained polymers were characterized by thermogravimetric analysis and the 10% weight loss temperatures of the poly(ester-imide)s were found to be in the range between 451 and 482 °C in nitrogen. Furthermore, crystallinity of the polymers was estimated by means of wide-angle X-ray diffraction. 相似文献
14.
Enthalpies for the two proton ionizations of the biochemical buffers N-[2-hydroxyethyl]piperazine-N′-[2-ethane sulfonic acid] (HEPES) and N-[2-hydroxyethyl]piperazine-N′-[2-hydroxypropane sulfonic acid] (HEPPSO) were obtained in water-methanol mixtures with methanol mole fraction (Xm) from 0 to 0.360. With increasing methanol, the ionization enthalpy for the first proton (ΔH1) of HEPES increased steadily from 8.4 to 15.3 kJ mol−1 whereas that for HEPPSO rose to a maximum of 21.0 kJ mol−1 at Xm = 0.123 before dropping to 18.4 kJ mol−1 at Xm = 0.360. The ionization enthalpy for the second proton (ΔH2) of HEPES varied from 20.8 kJ mol−1 in water to 13.6 kJ mol−1 at Xm = 0.360 with a maximum of 24.8 kJ mol−1 at Xm = 0.194. For HEPPSO, ΔH2 increased steadily from 23.4 to 29.2 kJ mol−1. The solvent composition was selected so as to include the region of maximum structure enhancement of water by methanol. The results were interpreted in terms of solvent-solvent and solvent-solute interactions. 相似文献
15.
Masahiro Yoshida Miki Shibata Saaya Mukae Kouki Kinoshita Kenji Matsumoto Tsukasa Hirokane 《Tetrahedron letters》2019,60(49):151262
Cyclization of 4-hydroxy-2-pyrones with allylic bisacetates by a palladium catalyst is described. Pyrone-annulated 2-oxabicyclo[3.3.1]nonane derivatives were regioselectively produced from the reaction of 4-hydroxy-2-pyrones with 1,4-diacetoxy-2-cyclohexene at high temperature. The reaction would proceed via a migration of the π-allylpalladium intermediate. 相似文献
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17.
The synthesis of some 7-substituted-3-azabicyclo[3.3.1]nonanes is described. Routes followed were the debenzoylation of the 7-benzoyl derivative 7 and the decarboxylation of the 7-carboxy compounds 21 and 27. The so-obtained 7-oxo-N-tosyl-3-azabicyclo[3.3.1]nonanes 8and 11 show an extremely low reactivity towards a series of nucleophilic reagents. From analysis of the 1H NMR spectral data of a series of derivatives, the twin-chain conformation for the 7-exo compounds and the chair-boat conformation for the 7-endo compounds is indicated. 相似文献
18.
An effective solid-phase preparation of the pharmaceutically interesting 4H-2-(3-hydroxy-4-methoxyphenyl)-naphtho[1,2-b]pyran-1-one system from an anchored bisarylacetylene is described. 相似文献
19.
Thermal reaction of 2-[N-(alk-2-enyl)benzylamino]-3-(2-substituted and 2,2-disubstituted)vinylpyrido[1,2-a]pyrimidin-4(4H)-ones gave azepine, the desired ene products, and/or pyran derivatives. The formation of the latter was responsible for the [4+2] cycloaddition reaction between the α,β-unsaturated ester carbonyl moiety as a diene part and the alkenylamino moiety as an ene one. The reaction features depended upon the kinds of substituents both on the vinyl and alkenyl counterparts; strongly electron-withdrawing substituents on the vinyl moiety or an electron-donating substituent on the alkenyl one changed the reaction feature from the ene reaction to the hetero Diels-Alder reaction. 相似文献
20.
A series of N-(2-pyridyl)benzamides (1)-(11) and their nickel complexes, [N-(2-pyridyl)benzamide]dinickel(II) di-μ-bromide dibromide (12)-(16) and (aryl)[N-(2-pyridyl)benzamido](triphenylphosphine)nickel(II) (17)-(24), were synthesized and characterized. The single-crystal X-ray analysis revealed that 12 and 14 are binuclear nickel complexes bridged by bromine atoms and each nickel atom adopts a distorted trigonal bipyramidal geometry. The key feature of the complexes 17, 19 and 23 is each has a six-membered nickel chelate ring including a deprotonated secondary nitrogen atom and an O-donor atom. The nickel complexes show moderate to high catalytic activity for ethylene oligomerization with methylaluminoxane (MAO) as cocatalyst. The activity of 12-16/MAO systems is up to 3.3 × 104 g mol−1 h−1 whereas for 17-24/MAO systems it is up to 4.94 × 105 g mol−1 atm−1 h−1. The influence of Al/Ni molar ratio, reaction temperature, reaction period and PPh3/Ni molar ratio on catalytic activity was investigated. 相似文献