Synthesis of N,N′-bis(2,4-dinitrobenzofuroxan)-1,3,5-trinitro-2,6-diaminobenzene

N,N′-bis(2,4-dinitrobenzofuroxan)-1,3,5-trinitro-2,6-diaminobenzene (V) has been synthesized from 1,3-diaminobenzene and trinitrodichlorobenzene. The molecular structure of this compound has been determined by elemental analysis, IR, ¹H-NMR, and MS spectroscopies.     

Synthesis and characterization of phosphorus-containing polyamides and copolyamides based on 1-[(dialkoxyphosphinyl) methyl]-2,4-and -2,6-diaminobenzenes

Phosphorus-containing polyamides and copolyamides were prepared from 1-[(dialkoxyphosphinyl)methyl]-2,4 - and -2,4-diaminobenzenes. The polymers were characterized by infrared and proton nuclear magnetic resonance spectroscopy. differential scanning calorimetry, and thermogravimetric analysis. Their thermal properties were compared with those of the corresponding common polyamides. In addition, the fire resistance of some polyamides was evaluated by determining their limiting oxygen index value.     

Studies on the curing kinetics and thermal stability of the novel tetrafunctional epoxy resin N,N,N′N′-tetrakis(2,3-epoxypropyl)-4,4′-(1,4-phenylenedioxy)dianiline

A novel tetrafunctional epoxy resin, namely N,N,N′N′-tetrakis(2,3-epoxypropyl)-4,4′-(1,4-phenylenedioxy)dianiline, has been synthesized. The curing kinetics has been studied by differential scanning calorimetry (DSC) using various amine curing agents. Thermal stabilities of the cured products have been investigated by thermogravimetric (TG) analyses. The overall activation energies for the curing reactions are observed to be in the range 63.6–196.7 kJ·mol^–1. The cured products have good thermal stability.     

N,N''-二(3,4-二甲氧基苄基)-1,2-乙二胺的合成研究

N，N′-二(3，4-二甲氧基苄基)-l，2-乙二胺是合成抗癌增效剂SDB-乙二胺等药物的重要中间体。通过研究确证了其真实结构，改进了提纯方法，提高了后续反应的收率。     

Synthesis of N,N′-Bis(2-Nitro-Benzodifuroxanyl)-1,3,5-Trinitro-2,6-Diaminobenzene

N,N′-Bis(2-nitro-benzodifuroxanyl)-1,3,5-trinitro-2,6-diaminobenzene has been synthesized from 1,3-diaminobenzene and trinitrotrichlorobenzene. The molecular structure of this compound has been determined by elemental analysis, IR, ¹HNMR, and MS spectroscopies.     

Properties of poly[N,N′-(4,4′-diphenyl ether) 4-amidophthalimide] film

A high molecular weight polyamide–imide polymer derived from the reaction of TMAC–DAPE has been prepared and its film properties have been evaluated. Poly-[N,N′-(4,4′-diphenyl ether) 4-amidophthalimide] film has an excellent combination of mechanical, electrical, and chemical properties at room temperature and at 200°C. A comparison of the film properties of this material with those of a commercial polyimide film, Teflon, FEP, Nomex paper, and Mylar films is also presented.     

Thermal properties of poly[N,N′-(4,4′-diphenyl ether) 4-amidophthalimide] film

The aging behavior of a polyamide–imide film was investigated. Film samples have been exposed to temperatures from 225° to 350°C for various times and the mechanical and electrical properties measured. This information was used to construct log life plots to gain an insight into the service life of this material. TGA and DTA results coupled with the information from the aging tests indicate that this film can be used at temperatures of 180° to 200°C for extended periods of time. Mechanical properties, especially elongation, of the film deteriorate faster than the electrical properties.     

Synthesis and characterization of aliphatic copolyesters containing 1,4‐bis[(carboxylethoxy)methyl]cyclohexane

A series of aliphatic copolyesters was synthesized using newly prepared cyclohexane‐based alicyclic diacid, succinic acid and 1,4‐butanediol with various molar ratios, in order to investigate the effects of these compositions on the crystallinity and thermal properties of the aliphatic copolyesters. The structures, average molecular weights and physical properties of the resulting random aliphatic copolyesters were characterized using nuclear magnetic resonance, gel permeation chromatography, differential scanning calorimetry (DSC) and X‐ray diffraction. The results of DSC reveal that thermal and crystallization behaviors depend on the corresponding diacid comonomer (1,4‐bis[(carboxylethoxy)methyl]cyclohexane) content in the aliphatic copolymers. However, the crystalline structures of the aliphatic copolyesters and of poly(butylene succinate) homopolymer are identical. Copyright © 2011 Society of Chemical Industry     

Study of reaction between N,N,N′,N′,N′-pentakis (hydroxymethyl) melamine and ethylene or propylene oxide

The effects of the kind and amount of oxirane (propylene or ethylene oxide), the amount of triethylamine catalyst, and the temperature on the reaction with N,N,N′,N′,N′-pentakis (hydroxymethyl) melamine (PHMM) in DMSO solution were studied. The changes in the content of reactive groups in the reaction mixture and in the final product were analyzed. The oxirane addition was shown to be accompanied by the condensation of hydroxymethyl groups in the PHMM. Optimal conditions for the synthesis and the structural formula of the s-triazine ring containing polyetherols were established. © 1997 John Wiley & Sons, Inc. J Appl Polym Sci 65: 2589–2602, 1997     

胺基甲基-4-硝基苯酚衍生物的合成研究

制备了四只 DIAR成色剂的定时基化合物,通过了红外、核磁、质谱对该化合物的结构及物理性质的测定。     

Zur Stereochemie von N,N′-Bis-[3-(o-ethoxyphenoxy)-2-hydroxy-propyl]-ethylendiamin

Stereochemistry of N,N′-Bis-[3-(o-ethoxyphenoxy)-2-hydroxy-propyl]-ethylendiamine N,N′-Bis-[3-(o-ethoxyphenoxy)-2-hydroxy-propyl]-ethylene diamine ( 5 ), synthesized from racemic 1,2-anhydro-3-O-(o-ethoxyphenyl)-glycerol ( 1 ) and ethylene diamine ( 2 ) or N,N′-dibenzyl ethylene diamine ( 3 ) crystallized in two fractions with different melting points. Both of these analytically pure products gave identical two spot tl-chromatograms on achiral phases. Attempts were made to resolve the mixtures which proved to consist of configurative but not constitutive isomers. Optically pure products were synthesized from chiral precursors.     

1-N-Boc-4-甲氨甲基哌啶合成方法

以4-哌啶甲酸为原料,经酯化、还原、(Boc)2O保护、溴代、甲胺化五步反应,以72%的总收率合成了重要药物中间体1-N-Boc-4-甲氨甲基哌啶。合成方法操作简单、收率高。     

N,N’-1,4-二对甲苯磺酰高哌嗪的合成

以甲醇钠为催化剂合成出N,N’-1,4-二对甲苯磺酰高哌嗪,考察了原料的物质的量比、反应时间、溶剂用量和相转移催化剂用量4种因素对反应收率的影响,较佳工艺条件为:N,N’-1,4-二对甲苯磺酰乙二胺0.02 mol时,N,N’-二对甲苯磺酰乙二胺和1,3-二溴丙烷的投料物质的量比1∶1.25,反应时间13 h,溶剂二甲基甲酰胺用量60 mL,苄基三乙基溴化铵用量0.6 g,总收率达65.65%。     

Synthesis,Structure, and Properties of N,N′‐Dinitrourea

Information on synthesis methods and properties of N,N′‐dinitrourea and its salts, which were reported virtually simultaneously by different authors in different publications, is summarized and systematized. Merits and drawbacks of various approaches for the synthesis of the target products are discussed. The reactivity of N,N′‐dinitrourea and its salts in the reactions of nucleophilic substitution and condensation is discussed.     

Antioxidants and stabilizers, 81. Transformations of N,N′-diphenyl- and N-phenyl-N′-isopropyl-1,4-benzoquinonediimines on silicagel

Transformations of N,N′-disubstituted 1,4-benzoquinonediimines have been investigated as a means for the elucidation of processes occurring in hydrocarbon polymers stabilized with amine antidegradants and of transformations accompanying the analyses of extracts of aged rubbers. N-Phenyl-N′-isopropyl-1,4-benzoquinonediimine (1b) is quickly hydrolyzed on a silicagel surface, giving rise to N-phenyl-1,4-benzoquinoneimine (3). The hydrolysis of N,N′-diphenyl-1,4-benzoquinonediimine (1a) proceeds more slowly under the same conditions, but the released aniline quickly reacts with the initial (1a), giving rise to N,N′-diphenyl-1,4-phenylenediamine(2a), 2-(phenylamino)-N,N′-diphenyl-1,4-benzoquinonediimine (4) and azophenine (5). The Reaction is catalyzed by the weakly acid surface of silicagel. Compound (4) is readily disproportionated thermally to 1,2,4-tris(phenylamino)-benzene (8) and 2, 10-dihydro-10-phenyl-2-(phenylimino)phenazine (9), even in the absence of a catalyst. A mechanism of the formation of compounds arising in the reaction has been suggested. Diimine (1a) possesses a higher oxidation potential than all the products derived from it, so that it is quickly reduced by these products to (2a). The gradual formation of (2a) may explain the retardation effects of (1a) in the autooxidation of hydrocarbon substrates.     

An NMR study of the dissociation of N,N′-(2-propyloximino)-4,4′-methylenebis(phenylcarbamate) and its crosslinking of polymers containing labile hydrogens. II

Nuclear magnetic resonance spectroscopy has been used to study the dissociation and reaction of N,N′-(2-propyloximino)-4,4′-methylenebis(phenylcarbamate), as a crosslinking agent for polymers containing labile hydrogens. The crosslinking of poly(acrylic acid), polyacrylamide, and poly(vinyl alcohol) was found to result upon heating each to 150°C for 10 min with this component at 2–10 wt %.     

Synthesis of N,N′ -Bis(2, 4-Dinitrobenzofuroxanyl)-3, 5-Dinitro-2, 6-Diaminopyridine

N,N′-Bis(2,4-dinitrobenzofuroxanyl) -3,5-dinitro-2,6-diaminopyridine has been synthesized from 2,6-diaminopyridine and trinitrodichlorobenzene. For this compound, the structure has been determined by elemental analysis, IR,¹HNMR and MS spectroscopies.     

N(2)-乙酰基-7-[(2-乙酰氧乙氧基)甲基]鸟嘌呤的转糖基作用

研究了N(2 ) 乙酰基 7 [(2 乙酰氧乙氧基 )甲基 ]鸟嘌呤通过转糖基作用生成其9位异构体N(2 ) 乙酰基 9 [(2 乙酰氧乙氧基 )甲基 ]鸟嘌呤的条件 ,转化率为 5 5 %。