Cyclization of N-(2,4,6-trimethylphenyl)-β-alanines

Reaction of 2,4,6-trimethylaniline with acrylic and itaconic acids gives the corresponding N-substituted =alanines which can be converted to derivatives of tetrahydropyridone, dihydropyrimidinedione, and 4-carboxy-2-pyrrolidinone. Bromination of the aromatic substituent in the synthesized heterocycles has been carried out.Kaunas Technological University, Kaunas 3028, Lithuania Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 7, pp. 951–954, July, 2000     

Synthesis and cyclization of N-(2-hydroxyphenyl)-and N-(2-benzyloxyphenyl)-Β-alanines

N-Substituted -alanines have been synthesized by treating o-aminophenol or o-benzyloxyaniline with acrylic, methacrylic, or crotonic acids. Their cyclization to 2-benzoxazolinones and dihydro-2,4(1H,3H)-pyrimidinediones has been studied.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 4, pp. 527–531, April, 1991.     

Crystal Structure of O,O'-Diphenyl N-(o-methylphenyl)-P-toluenesulfonamidomethylphosphonate

1INTR0DUCT10NThederivativesofaaminoph0sphonicacidhaveversatilebiologicalactivities-`13Inordertolookforhighlyeffectiveandselectivenewpesticides,aseriesofdiethyl1-(P-tohienesulfonamido)methylphosphonates1havebeensynthesizedbyathree-com-P0nentreacti0nofp-t0luenesulfonamide,formaldehydeandtriphenylphosphite.t2j'The1HNMRspectraoftheprbductsin-dicatethatthetwohydrogenatoms0ntheaCatomaremagneticallyequivalentwhenthesubstitutedgroupsonNatomareH,CH3andEt02CCHz'However,(R=H.Me,EtO,CCH,,o-me…     

改进Vilsmerier法合成4-(N-甲基,N-取代)氨基苯甲醛

以N-甲基,N-取代苯胺为原料,用环己烷作溶剂,以DMF和SOCl2替代经典的DMF和POCl3组成的Vilsmeier试剂,合成了5个4-(N-甲基,N-取代)氨基苯甲醛,确立了较优反应条件,一次收率达85~91%,溶剂可循环利用。对合成目标化合物进行了IR,1HNMR结构表征。     

Thermal Behavior of N,N''''-Bis[N-(2,2,2-trinitroethyl)- N-nitro]ethylenediamine

Introduction N,N'-Bis[N-(2,2,2-trinitroethyl)-N-nitro]ethyenedi- amine (BTNEDA) is a typical nitramine compound, which is structurally shown in Figure 1. The crystal density is 1.87 gcm-3. The detonation velocity corresponding to r=1.842 gcm-3 is about 8970 ms-1.1 Therefore, BTNEDA is used as high explosive. Its thermogram has been reported.2 In this paper, its kinetic parameters of the exothermic decomposition reaction are described. This is quite useful in the evaluation of its ther…     

一种新的选择性氧化苏-(1S,2S)-2-(N,N-二甲胺基)-1-(对硝基苯基)-1,3-丙二醇的N-甲基为N-甲酰基的方法

报告多官能团化合物苏 (1S ,2S) 2 (N ,N 二甲胺基 ) 1 (对硝基苯基 ) 1,3 丙二醇与聚合物支载条件下的溴试剂发生的一种新的选择性N 甲基氧化为N 甲酰基的反应 .在Na2 HPO4存在下 ,苏 (1S ,2S) 2 (N ,N 二甲胺基 ) 1 (对硝基苯基 ) 1,3 丙二醇于水 CCl4体系中被 717阴离子交换树脂支载的溴在 60℃氧化 2 4h给出 5 1%收率的苏 (1S ,2S) 2 (N 甲基 N 甲酰胺基 ) 1 (对硝基苯基 ) 1,3 丙二醇 .这种选择性N 甲基氧化为N 甲酰基的反应在 2 氨基 1,3 丙二醇衍生物化学中是第一次观察到 .     

Kinetics and mechanism of mercuration of N-(substituted benzylidene)-4-toluidines

In order to investigate the mechanism of mercuration reaction of substituted ben-zylideneanilines, kinetic measurements of these reactions at different temperatures (40-60℃) inmethanol-l,4-dioxane (1/1, V/V) were carried out and Hammett ρ value for C-phenyl substituentsof-0.61 for the N-(substituted benzylidene)-4-toluidine series was obtained. Thermodynamicparameters E_a, △S~≠ were obtained for the reaction of different. N-(substituted benzylidene)-4-toluidines. It was found that this ortho-mercuration was brought about by an internal cyclometal-lation process involving the imino-moiety.     

Crystal structure of N-(β-acetoxyethyl)-4-methylpyridinium bromide

In continuation of previous studies [1] on structures of compounds differing from acetylcholine and choline by having a pyridine ring instead of the quaternary N atom, the x-ray structure of N-(-acetoxyethyl)-4-methylpyridinium bromide, which has cholinergic activity [2], is solved.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 8, pp. 1813–1816, August, 1991.     

Synthesis and Cyclization of N-(4-Phenoxyphenyl)-β-alanines

We have used the reaction of 4-aminodiphenyl ester with acrylic, methacrylic, crotonic, and itaconic acids to synthesize N-substituted -alanines, which undergo ring closure to form derivatives of dihydropyrimidinedione and 4-carboxy-2-pyrrolidinone. We have studied the reactions of acylation and recyclization of the dihydropyrimidinedione ring, and we have synthesized derivatives of 4-carboxy-1-(4-phenoxyphenyl)-2-pyrrolidinone: arylidene hydrazides, 2[(2-oxo-4-pyrrolidinyl-1-(4-phenoxyphenyl)]benzimidazole.     

N-(3-十六烷氧基-2-羟基丙基)-N,N-二甲基甜菜碱的制备

以十六醇、环氧氯丙烷、二甲胺和氯乙酸钠等为原料,通过三步反应合成N-(3-十六烷氧基-2-羟基丙基)-N,N-二甲基甜菜碱(HHDB),并探索了反应温度、投料比、反应时间和催化剂等因素对产物产率的影响,确定了最佳反应条件。中间体3-十六烷氧基-2-羟基-1-氯丙烷(HHCP)合成的最佳工艺条件:催化剂苄基三乙基氯化铵,体系p H为9.0,n(C_(16)H_(33)OH)∶n(C_3H_5OCl)=1∶1.1,滴加环氧氯丙烷温度65℃,滴加时间1.5h,反应温度95℃,反应时间5 h;中间体N-(3-十六烷氧基-2-羟基丙基)-N,N-二甲基叔胺(HHDT)合成的最佳工艺条件:n(C_(19)H_(39)OCl)∶n(C_2H_7N)=1∶1.2,反应温度85℃,反应时间20 h;产物HHDB制备的最佳工艺条件:n(C_(21)H_(45)ON)∶n(C_3H_4O_2ClNa)=1∶1.1,反应温度80℃,反应时间4 h。在上述工艺条件下,HHDB产率达到95.2%,对产物HHDB及中间体进行红外光谱与核磁氢谱表征,测定其临界胶束浓度为9.8 mmol·L-1,水溶液表面张力为18.8 m N·m-1,发泡力为1.15,产物具有较好的表面活性。     

Evaluation of Transient Absorption Spectra of N, N, N, N- Tetra - ( p -methylphenyl ) - 4, 4- diamino - 1, 1- diphenyl Ether ( TPDAE ) for Electron Transfer from TPDAE to Fullerenes ( C_(60) / C_(70) ) by Laser Flash Photolysis

Fullerenes C60 and C70 have high electron affinity ( 2.6 - 2.8 ev ) and readily form anions on electronchemical reduction1, which were famous as electron acceptor in photo-excitation because of symmetrical shape, large size, and properties of its p - electron system2. After observation of molecular ferromagnetism3 in the tetrakis (dimethylamino ) ethylene salt of C60 as well as the occurrence of ultra-fast photoinduced electron transfer within the dimethyl aniline - C60 complex4, prompted us…     

Features of the reactions of β-aryl(heteryl)-α-nitroacrylates with N,N-, N,O-, and N,S-binucleophiles

The reactions of ??-aryl(heteryl)-??-nitroacrylates with N,N-, N,O-, and N,S-binucleophiles proceed regiospecifically through the initial formation of the Ad_N products, among which only the product from o-aminothiophenol was isolated. The conditions of converting the S-adducts into 2-aryl(heteryl)benzothiazole were found. The N-adducts formed in the reaction with hydrazine, o-phenylenediamine, and o-aminophenol undergo immediately the spontaneous transformation into the linear (azine, azomethine) or heterocyclic (benzimidazole) structures.     

Synthesis of N-(alkoxycarbonyl or alkoxycarbonyl-methyl-alkoxyphosphonyl)-α-amino-O,O-diphenyl phosphonates and their bioactivities

With phosphoric formic acid (PFA) and its analog,phosphonoacetic acid (PAA),as the lead compounds,α-amino phosphonates were introduced into PFA and PAA.The derivatives oi N-( alkoxycarbonyl-aikoxyphosphonyl)-α-arnino phosphonates (Ⅰ) and N-(alkoxycarbonyl-methyt-alkoxyphosphonyl)-α-amino phosphonates (Ⅱ) with the N-terminal of amino phosphonates bonding to phosphorus atom of PFA and PAA were synthesized via the reaction of the corresponding phosphonyl chloride with a-amino phosphonates in the presence of a base.The 31P NMK spectra of Ⅰ and Ⅱwere determined.It is found that the coupling constants 3Jpp with R3 being alkyl group were lower than those with R3 being (substituted) phenyl,and this result was discussed.The preliminary bioassay showed that some of the compounds Ⅰ and Ⅱhave better activities against tobacco mosaic virus (TMV).The inhibitory was higher than that of DHT (2,4-dioxyhexahydro-1,3,5-triazine).In addition,some of the compounds showed the activity against cancer cells.     

Crystal Structure of N-(O-Ethylphenylthionophos-phonyl) N'-(O-p-iodinephenylphenylthionophos-phonyl)thiosemicarbazide

1mThODUCT'ONSomecomPOundsofN--thionophosphonylandN,N'--his(thionophosphonyl)thiOSemicarbazideshaveattractedmuchattentionandbeenextensivelystudiedinrecentyears"~'i.ThiskindofcomPOundsareknowntohaveobviousantibacterialandantifungalactivitiest3}.TherearetwochiralphosphoratomsinthecomPOundsofN,N'--his(thionophosphonyl)thiosemicarbazide.Inordertostudyfurthertherelationshipbetweenthestructureandbiologicalactivities,hereinwerePOrtthecrystalstructureofakindofN,N'--his(thionophosphonyl)thiose…     

Au(III)-catalyzed tandem amination-hydration of alkynes: synthesis of α-(N-2-pyridonyl)ketones

A new Au(III)-catalyzed tandem amination-hydration reaction has been discovered, leading to the formation of α-(N-2-pyridonyl)ketones and heterocyclic analogues in good to excellent yields (14 examples, 48-90%). This reaction demonstrates the unusual use of a heterocyclic sp(2) nitrogen nucleophile in a gold-catalyzed 6-endo-dig cyclization. The tandem process allows rapid access to α-(N-2-pyridonyl)ketones, making them a convenient building block for the synthesis of more complex N-alkyl pyridone targets.     

Behavior of double stimuli-responsive copolymer of N-(3-(diethylamino) propyl)-N-methylacrylamide and N,N–diethylacrylamide in aqueous solutions

Double stimuli-responsive copolymer of N-(3-(diethylamino)propyl)-N-methylacrylamide and N,N-diethylacrylamide (molar mass M ≈ 32,000?g?mol^?1) in buffer solutions was studied by the static and dynamic light scattering and turbidimetry. The experiments were performed within pH interval from 7 to 13 and in a wide concentration range. Two types of scattering species were observed in solutions of all concentrations and pH at room temperatures. They were macromolecular unimers and loose aggregates. The increase in concentration and pH led to decrease in phase separation temperatures and width of phase transition.     

Synthesis and Characterization of N-(2,2-Diphenylacetyl)- N′-Substituted Thiourea Derivatives: The Crystal Structure of N-(2,2-Diphenylacetyl)-N′-(4-chloro phenyl)-thiourea

A series of new N-(2,2-diphenylacetyl)-N ′-substituted thiourea derivatives (1–9) have been prepared and characterized by elemental analyses, IR and ¹H NMR spectroscopy. N-(2,2-diphenylacetyl)-N ′-(4-chlorophenyl)-thiourea was also characterized by a single crystal X-ray diffraction study. The compound crystallizes in the monoclinic space group P2₁/c with Z = 4 and a = 9.6551(19) Å, b = 20.060(4) Å, c = 9.894(2) Å, β = 104.29(3)°. The molecular conformation of the compound is stabilized by an intramolecular (N1-H1···O1) hydrogen bond that forms a pseudo-six-membered ring.