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1.
《高分子科学杂志,A辑:纯化学与应用化学》2013,50(8):889-896
Abstract Electrophilic trisubstituted ethylenes, ring‐substituted ethyl 2‐cyano‐3‐phenyl‐2‐propenoates, RC6H4CH?C(CN)CO2C2H5 (where R is 2‐CH3, 3‐CH3, 4‐CH3, 2‐OCH3, 3‐OCH3, and 4‐OCH3) were prepared and copolymerized with styrene (ST). The monomers were synthesized by the piperidine catalyzed Knoevenagel condensation of ring‐substituted benzaldehydes and ethyl cyanoacetate, and characterized by CHN analysis, IR, 1H and 13C NMR. All the ethylenes were copolymerized with ST (M1) in solution with radical initiation (AIBN) at 70°C. The compositions of the copolymers were calculated from nitrogen analysis and the structures were analyzed by IR, 1H and 13C NMR. The order of relative reactivity (1/r 1) for the monomers is 3‐OCH3 (0.88)?>?4‐CH3 (0.71)?>?2‐OCH3 (0.68)?>?3‐CH3 (0.55)?>?2‐CH3 (0.47)?>?4‐OCH3 (0.40). Higher T g of the copolymers in comparison with that of polystyrene indicates a decrease in chain mobility of the copolymer due to the high dipolar character of the TSE structural unit. Gravimetric analysis indicated that the copolymers decompose in the 257–287°C range. 相似文献
2.
A general method for the preparation of 2‐(N‐Substituted)‐2‐imidazolines and 2‐(N‐Substituted)‐1,4,5,6‐tetrahydropyrimidines is described. These heterocycles can be synthesized from their respective anilines with 2‐chloro‐2‐imidazoline or 2‐chloro‐1,4,5,6‐tetrahydropyrimidine, generated in situ from imidazolidin‐2‐one and tetrahydropyrimidin‐2(1H)‐one activated by dimethyl chlorophosphate, in good to excellent yields. 相似文献
3.
General and Facial Synthesis of 2‐Amino‐5‐halogenpyrimidine‐4‐carboxylic Acids and Their Derivatives
A facile synthetic approach to 2‐amino‐5‐halogen‐pyrimidine‐4‐carboxylic acids from 5‐halogen‐2‐methylsulfonylpyrimidine‐4‐carboxylic acid by nucleophilic displacement of the methylsulfonyl group with primary and secondary aliphatic amines has been developed. The titled amino acids underwent decarboxylation, yielding 2‐amino‐5‐halogenpyrimidines. Starting from 2‐amino‐5‐chloropyrimidine‐4‐carboxylic acid chlorides, 2‐[5‐chloro‐2‐(amino)‐4‐pyrimidinyl]‐2‐oxo‐1‐(2‐pyridyl)‐ethyl cyanides were obtained in excellent yields. 相似文献
4.
Gregory B. Kharas Maria R. Cisneros Mollie E. Buchmann Ana Maria Gallegos Matthew J. Hurzeler Jason W. Karras 《高分子科学杂志,A辑:纯化学与应用化学》2013,50(6):865-870
Electrophilic trisubstituted ethylene monomers, alkyl ring substituted methyl 2‐cyano‐3‐phenyl‐2‐propenoates, RC6H4CH[dbnd]C(CN)CO2CH3, where R is 2‐methyl, 3‐methyl, 4‐methyl, 4‐isopropyl, and 2,5‐dimethyl were synthesized by piperidine catalyzed Knoevenagel condensation of ring‐substituted benzaldehydes and methyl cyanoacetate, and characterized by CHN elemental analysis, IR, 1H and 13C NMR. Novel copolymers of the ethylenes and styrene were prepared at equimolar monomer feed composition by solution copolymerization in the presence of a radical initiator (AIBN) at 70°C. The composition of the copolymers was calculated from nitrogen analysis, and the structures were analyzed by IR, 1H and 13C NMR, GPC, DSC, and TGA. High Tg of the copolymers in comparison with that of polystyrene indicates a substantial decrease in chain mobility of the copolymer due to the high dipolar character of the trisubstituted ethylene monomer unit. The gravimetric analysis indicated that the copolymers decompose in the 260–400°C range. 相似文献
5.
《高分子科学杂志,A辑:纯化学与应用化学》2013,50(8):957-962
Equimolar alternating copolymers of vinyl acetate and electrophilic trisubstituted ethylene monomers, ring‐substituted methyl (E)‐2‐cyano‐3‐phenyl‐2‐propenoates, RC6H4CH?C(CN)CO2CH3 (where R=4‐acetamido, 2‐cyano, 3‐cyano, 4‐cyano, 4‐diethylamino) were prepared via copolymerization in solution with radical initiation (ABCN) at 70°C. The compositions of the copolymers were calculated from nitrogen analysis and the structures were analyzed by IR, 1H‐ and 13C‐NMR. High glass transition temperatures of the copolymers in comparison with that of polyvinyl acetate indicate a decrease in chain mobility of the copolymers due to the high dipolar character of the trisubstituted ethylene monomer unit. The gravimetric analysis indicated that the decomposition of the copolymers occurs in two steps. The first step is relatively fast weight loss in 257–370°C range followed by very slow decomposition of the formed residue in 370–950°C range. 相似文献
6.
A. M. Astakhov A. D. Vasil'ev M. S. Molokeev Yu. V. Kekin L. A. Kruglyakova R. S. Stepanov 《Journal of Structural Chemistry》2003,44(2):326-329
An Xray structural investigation of 2nitro1ureidoguanidine has been carried out. The crystals are monoclinic: a = 4.4690(2), b = 15.566(1), c = 9.4131(7), = 94.896(5)°, V = 652.4(3)>
3, space group P21/n, Z = 4, calc = 1.650 g/cm3. The molecule consists of two planar fragments: carbamide and nitroguanidine. The geometrical characteristics of the molecule are analyzed. The system of intra and intermolecular hydrogen bonds in the crystal is considered. 相似文献
7.
Svetlana A. Burova Russ N. Fitzgerald Byron S. Johnson Richard T. Matsuoka 《合成通讯》2013,43(18):3029-3039
A novel method for preparation of 1‐substituted benzimidazoles via reductive amination of ketones with N‐differentiated 1,2‐diaminobenzenes is described. The method appears to be general in application to acyclic and cyclic ketones, as well as heteroatom‐substituted cyclic ketones. 相似文献
8.
Shashikanth Ponnala 《合成通讯》2013,43(15):2189-2194
2‐Arylbenzoxazoles and 2‐arylbenzimidazoles were synthesized by the reaction of aldehydes with 2‐aminophenol and O‐phenylenediamines in the presence of iodine. 1,3,5‐Trisubstituted pyrazoles were synthesized from chalcones and hydrazines in the presence of iodine. 相似文献
9.
Gregory B. Kharas Xue Tian Joanna Alegarbes Andrea T. Bartosik Mirela Hadziahmetovic Asra K. Hai 《高分子科学杂志,A辑:纯化学与应用化学》2013,50(6):565-568
Electrophilic trisubstituted ethylene monomers, ring‐substituted 2‐cyano‐N,N‐dimethyl‐3‐phenyl‐2‐propenamides, RC6H4CH?C(CN)CON(CH3)2 (where R is 3‐benzyloxy, 4‐benzyloxy, 3‐ethoxy‐4‐methoxy, 3‐bromo‐4‐methoxy, 5‐bromo‐2‐methoxy, 2‐chloro‐6‐fluoro) were synthesized by potassium hydroxide catalyzed Knoevenagel condensation of ring‐substituted benzaldehydes and N,N‐dimethyl cyanoacetamide, and characterized by CHN elemental analysis, IR, 1H‐ and 13C‐NMR. Novel copolymers of the ethylenes and styrene were prepared at equimolar monomer feed composition by solution copolymerization in the presence of a radical initiator, ABCN at 70°C. The composition of the copolymers was calculated from nitrogen analysis, and the structures were analyzed by IR, 1H and 13C NMR, GPC, DSC, and TGA. High Tg of the copolymers in comparison with that of polystyrene indicates a substantial decrease in chain mobility of the copolymer due to the high dipolar character of the trisubstituted ethylene monomer unit. The gravimetric analysis indicated that the copolymers decompose in the 300–450°C range. 相似文献
10.
《合成通讯》2013,43(15):2067-2077
Abstract We have synthesized and characterized a series of alkyl and aryl‐(4‐methyl‐6‐nitro‐quinolin‐2‐yl)amines through a high‐yield, three‐step procedure starting from 4‐methylquinolin‐2‐ol. Nitration using concentrated nitric/sulfuric acids, followed by chlorination in phosphorus oxychloride, yielded 2‐chloro‐4‐methyl‐6‐nitro‐quinoline. All of the intermediates and aminated products have been characterized by multinuclear (1H and 13C) NMR spectroscopy, elemental analysis, and, in the case of the two title compounds (ethyl and cyclohexyl‐(4‐methyl‐6‐nitro‐quinolin‐2‐yl)amine), a single crystal X‐ray structure was obtained to verify the nature of the new materials. 相似文献
11.
Gregory B. Kharas Xue Tian Traci A. Ackron Michael H. Akroush Kelly A. O'brien Ella Ostrovskaya 《高分子科学杂志,A辑:纯化学与应用化学》2013,50(3):243-247
Electrophilic trisubstituted ethylene monomers, halogen ring‐substituted 2‐cyano‐N,N‐dimethyl‐3‐phenyl‐2‐propenamides, RC6H4CH [dbnd]C(CN)CON(CH3)2 (where R is 2‐Br, 3‐Br, 4‐Br, 2‐Cl, 3‐Cl, 4‐Cl, 2‐F, 3‐F, 4‐F), were synthesized by potassium hydroxide catalyzed Knoevenagel condensation of ring‐substituted benzaldehydes and N,N‐dimethyl cyanoacetamide, and characterized by CHN elemental analysis, IR, 1H‐ and 13C‐NMR. Novel copolymers of the ethylenes and styrene were prepared at equimolar monomer feed composition by solution copolymerization in the presence of a radical initiator, ABCN at 70°C. The composition of the copolymers was calculated from nitrogen analysis, and the structures were analyzed by IR, 1H and 13C NMR, GPC, DSC, and TGA. High T g of the copolymers in comparison with that of polystyrene indicates a substantial decrease in chain mobility of the copolymer due to the high dipolar character of the trisubstituted ethylene monomer unit. The gravimetric analysis indicated that the copolymers decompose in the 300–450°C range. 相似文献
12.
This report describes the synthesis of 4‐substituted‐ and 1,4‐disubstituted‐4‐hydroxypyrrolidin‐2‐ones by cyclization of intermediate γ‐aminoesters prepared from alkylbenzylamines, α‐bromoketones, and lithio ethyl acetate. 相似文献
13.
The anomerically pure benzyl α‐d‐glycoside of 2‐amino‐2‐deoxy‐mannopyranoside was synthesized from d‐glucopyranose via 2‐amino‐2‐deoxy‐d‐altrose intermediates. Unlike the direct synthesis from mannosamine in the literature, our method provides furanose‐free products. A new method for the preparation of cis‐2,3‐oxazolidinones of 2‐amino‐2‐deoxy‐sugars was developed. A selective removal of the glycosidic benzyl group in the presence of 4,6‐O‐benzylidene protection was developed, which may provide new routes for the synthesis of oligosaccharides. Furanose‐free derivatives of α‐benzyl‐2‐amino‐2‐deoxy‐mannopyranuronic acids synthesized here offered possibilities for direct comparisons to prior literature preparations. 相似文献
14.
Gregory B. Kharas Xue Tian Whitney K. Castle Marie B. Cuison Maria R. Fath Bridget Nord 《高分子科学杂志,A辑:纯化学与应用化学》2013,50(4):355-358
Electrophilic trisubstituted ethylene monomers, ring‐substituted 2‐cyano‐N,N‐dimethyl‐3‐phenyl‐2‐propenamides, RC6H4CH?C(CN)CON(CH3)2 (where R is 4‐(CH3)2N, 4‐CH3CO2, 4‐CH3CONH, 2‐CN, 3‐CN, 4‐CN, 4‐(C2H5)2N) were synthesized by potassium hydroxide catalyzed Knoevenagel condensation of ring‐substituted benzaldehydes and N,N‐dimethyl cyanoacetamide, and characterized by CHN elemental analysis, IR, 1H‐ and 13C‐NMR. Novel copolymers of the ethylenes and styrene were prepared at equimolar monomer feed composition by solution copolymerization in the presence of a radical initiator, ABCN at 70°C. The composition of the copolymers was calculated from nitrogen analysis, and the structures were analyzed by IR, 1H and 13C NMR, GPC, DSC, and TGA. High Tg of the copolymers in comparison with that of polystyrene indicates a substantial decrease in chain mobility of the copolymer due to the high dipolar character of the trisubstituted ethylene monomer unit. The gravimetric analysis indicated that the copolymers decompose in the 300–450°C range. 相似文献
15.
Novel Copolymers of Styrene and Alkoxy Ring‐Substituted 2‐Cyano‐N,N‐Dimethyl‐3‐Phenyl‐2‐Propenamides
Gregory B. Kharas Xue Tian Adam C. Hermsen Aditi S. Jani Larissa I. Kozij Emira Hadziahmetovic 《高分子科学杂志,A辑:纯化学与应用化学》2013,50(10):1485-1492
Electrophilic trisubstituted ethylene monomers, alkoxy ring‐substituted 2‐cyano‐N,N‐dimethyl‐3‐phenyl‐2‐propenamides, RC6H4CH?C(CN)CON(CH3)2 (where R is 2‐OCH3, 3‐OCH3, 4‐OCH3, 2‐OCH2CH3, 3‐OCH2CH3, 4‐OCH2CH2CH3, 4‐OCH2CH2CH2CH3), were synthesized by potassium hydroxide catalyzed Knoevenagel condensation of ring‐substituted benzaldehydes and N,N‐dimethyl cyanoacetamide, and characterized by CHN elemental analysis, IR, 1H‐ and 13C‐NMR. Novel copolymers of the ethylenes and styrene were prepared at equimolar monomer feed composition by solution copolymerization in the presence of a radical initiator, ACBN at 70°C. The composition of the copolymers was calculated from nitrogen analysis, and the structures were analyzed by IR, 1H and 13C NMR, GPC, DSC, and TGA. High Tg of the copolymers in comparison with that of polystyrene indicates a substantial decrease in chain mobility of the copolymer due to the high dipolar character of the trisubstituted ethylene monomer unit. The gravimetric analysis indicated that the copolymers decompose in the 300–450°C range. 相似文献
16.
Gregory B. Kharas Xue Tian Trang H. Huynh Thomas W. Lyons Lani A. Macartney Dylan Smith 《高分子科学杂志,A辑:纯化学与应用化学》2013,50(5):469-473
Electrophilic trisubstituted ethylene monomers, halogen ring‐disubstituted 2‐cyano‐N,N‐dimethyl‐3‐phenyl‐2‐propenamides, RC6H3CH?C(CN)CON(CH3)2 (where R is 2,3‐dichloro, 2,4‐dichloro, 2,6‐dichloro, 3,4‐dichloro, 3,5‐dichloro, 2,3‐difluoro, 2,4‐difluoro, 2,6‐difluoro, 3,4‐difluoro, 3,5‐difluoro), were synthesized by potassium hydroxide catalyzed Knoevenagel condensation of ring‐substituted benzaldehydes and N,N‐dimethyl cyanoacetamide, and characterized by CHN elemental analysis, IR, 1H‐ and 13C‐NMR. Novel copolymers of the ethylenes and styrene were prepared at equimolar monomer feed composition by solution copolymerization in the presence of a radical initiator, ABCN at 70°C. The composition of the copolymers was calculated from nitrogen analysis, and the structures were analyzed by IR, 1H and 13C NMR, GPC, DSC, and TGA. High Tg of the copolymers in comparison with that of polystyrene indicates a substantial decrease in chain mobility of the copolymer due to the high dipolar character of the trisubstituted ethylene monomer unit. The gravimetric analysis indicated that the copolymers decompose in the 300–450°C range. 相似文献
17.
18.
A convenient, five‐step preparation of 2‐acetyl‐4,5‐difluorothiophene from 2,3‐dibromothiophene is described. 相似文献
19.
2‐Aryl‐substituted nitriles were prepared in good to excellent yields in a one‐pot reaction by the reaction of benzyne, generated using neutral conditions from (phenyl)[o‐(trimethylsilyl)‐phenyl]iodonium triflate, and 2‐lithionitriles. 3‐Keto nitriles substituted at the 2‐position were obtained in good yields when these reactions were trapped with acid chlorides. The mechanism of the benzyne reaction in terms of a N‐lithiobenzocyclobutanimine intermediate is discussed. 相似文献
20.
Gregory B. Kharas Laura B. Passe Elizabeth Bishop Allison Dusinski Piran Farhadieh Mark Gatz 《高分子科学杂志,A辑:纯化学与应用化学》2013,50(8):779-782
Electrophilic trisubstituted ethylene monomers, ring‐substituted 2‐phenyl‐1,1‐dicyanoethylenes, RC6H4CH?C(CN)2 (where R is 2‐methoxy, 3‐methoxy, 4‐methoxy, 4‐ethoxy, 4‐propoxy, and 4‐butoxy), were synthesized by piperidine catalyzed Knoevenagel condensation of ring‐substituted benzaldehydes and malononitrile, and characterized by CHN elemental analysis, IR, 1H‐ and 13C‐NMR. Novel copolymers of the ethylenes and styrene were prepared at equimolar monomer feed composition by solution copolymerization in the presence of a radical initiator (AIBN) at 70°C. The composition of the copolymers was calculated from nitrogen analysis, and the structures were analyzed by IR, 1H and 13C NMR, GPC, DSC, and TGA. High T g of the copolymers in comparison with that of polystyrene indicates a substantial decrease in chain mobility of the copolymer due to the high dipolar character of the trisubstituted ethylene monomer unit. The gravimetric analysis indicated that the copolymers decompose in the 290–450°C range. 相似文献