二羧酸基取代三环氮杂冠醚的合成及其晶体结构

合成了一种新型的三环氮杂冠醚4,13-二氧-1,7,10,16-四氮-1,16：7, 10-双亚乙基-9,18-二乙酸环十八烷-8,17-二酮（C_(20)H_(32)H_4O_8）,在无 水乙醇-氯仿混合溶剂中培养出单晶,用X射线衍射法测定了晶体结构。该晶体属单 斜晶系,空间群P2_1/c,晶胞参数a = 0.87474(17) nm,b = 1.3967(3) nm,c = 0.94309(19) nm;β = 111.18(3)°;Z = 4,V = 1.0744(4) nm~3,D_c = 1. 411 g/cm~3,μ = 0.110 mm~(-1),F(000) = 488,R_1 = 0.0678,wR_2 = 0. 1850。     

Synthesis of Aromatic Amino Acid Amides

Aromatic amino esters, in toluene or water, react with aqueous ammonium hydroxide to give moderate to high yields of the corresponding amides.     

Synthesis and Rearrangement of N-PIII-Phosphorylated Carboxylic Acid Amides

Abstract

Reactions of carboxylic acid lactams with tervalent phosphorus chlorides, leading to N- and/or O- derivatives have been investigated. Synthetic methods for imidoylphosphites and phosphonates, mono- and bisphosphorylated azadienes have been developed. Prototropic migrations in azaallylic triad, phosphorus atom migrations in N-C-O triad and imidoylphosphite-imidoylphosphonate rearrangement were found. It was encountered, that chlorination of amidophosphites containing one to three trihalogen acetamide groups is accompanied by chlorine or N-acylamide group shift and leads to cyclic and spirocyclic phosphoranes with 1,3,2-⁵-oxazaphosphetanic cycle.     

三元环氨基酸的合成工艺改进

以甘氨酸乙酯盐酸盐为原料,经酰氨化、脱水、成环、水解反应合成了三元环氨基酸,总收率达50.4%。其结构经1HNMR,13CNMR,IR和EI-MS确证。     

Synthesis, Structure, and Membrane Activity of New Glycyrrhetic Acid Derivatives

Derivatives of 3-O-acetyl-18-H-glycyrrhetic acid were synthesized. Their structures and membrane activities were studied.     

4-Hydroxyquinolin-2-ones. 45. Synthesis, Structure, and Biological Activity of N-Substituted 1H-4-Hydroxy-2-oxoquinoline-3-acetic Acid Amides

A preparative method is proposed for obtaining N-substituted 1H-4-hydroxy-2-oxoquinoline-3-acetic acid amides. X-Ray diffraction analysis of one of the synthesized compounds has been carried out. The effect of the obtained substances on thyroid gland function has been studied.     

Synthesis, Structure and Catalytic Activity Comparison of Tris- and Tetracoordinated Lanthanide Amides

Tetracoordinated lanthanide amides [(MeaSi)2N]3Ln (μ-C1)Li(THF)3 (Ln=La (1), Pr (2)) were synthesized by the reaction of anhydrous lanthanide(Ⅲ) chlorides LnCl3 (Ln=La, Pr) with 3 equiv, of lithium bis(trimethylsilyl)amide (Me3Si)2NLi in THF, followed by recrystallization from toluene. Sublimation of 1 and 2 afforded the triscoordinate lanthanide amides [(Me3Si)2N]3Ln (Ln=La, Pr). The crystal structure of 2 was determined by X-ray diffraction analysis. The catalytic activity studies show that the tetracoordinate amides can be used as single-component MMA (methyl methacrylate) polymerization catalysts, while the triscoordinate amides showed poor activity on MMA polymerization under the same conditions.     

Synthesis,Structure, and Antimalarial Activity of Tricyclic 1,2,4-Trioxanes Related to Artemisinin

Two sets of tricyclic 1,2,4-trioxanes containing the ABC ( 10 , 11 ) and ACD ring portions ( 21 , 22 , 32 , 33 , 37 , and 38 ) of artemisinin ( 1 ) were synthesized by successive photo-oxygenation of appropriate enol-ether precursors to 1,2-dioxanes and inter- and intramolecular reaction with a carbonyl compound or oxo-substituted side-chain. The structures of 10 , 21 , and 22 were determined by X-ray analysis. The anti-malarial activity of all trioxanes, except 37 and 38 , was evaluated in vitro against chloroquine-sensitive and chloroquine-resistant Plasmodium falciparum parasites. Trioxanes 11 and 21 were as active as artemisinin ( 1 ). It was found that neither the lactone function nor rings B and D of 1 were essential for activity. A possible pharmacophore for artemisinin-like activity, which embodies a spirocyclopentane group attached to C(3) of 1,2,4-trioxane, was proposed.     

Synthesis of 4,5-Dichloroisothiazole-3-carboxylic Acid Amides and Esters

Previously unknown 4,5-dichloroisothiazole-3-carboxylic acid amides and esters were synthesized by reactions of 4,5-dichloroisothiazole-3-carbonyl chloride with ammonia, heterocyclic and aromatic amines, and functionally substituted alcohols and phenols.     

Synthesis,Photoisomerization, Antioxidant Activity,and Lipid-Lowering Effect of Ferulic Acid and Feruloyl Amides

The Ugi four-component reaction employing naturally occurred ferulic acid (FA) is proposed as a convenient method to synthesize feruloyl tertiary amides. Applying this strategy, a peptoid-like derivative of ferulic acid (FEF77) containing 2 additional hydroxy-substituted aryl groups, has been synthesized. The influence of the configuration of the double bond of ferulic acid and feruloyl amide on the antioxidant activity has been investigated thanks to light-mediated isomerization studies. At the cellular level, both FA, trans and cis isomers of FEF77 were able to protect human endothelial cord vein (HECV) cells from the oxidative damage induced by exposure to hydrogen peroxide, as measured by cell viability and ROS production assays. Moreover, in steatotic FaO rat hepatoma cells, an in vitro model resembling non-alcoholic fatty liver disease (NAFLD), the molecules exhibited a lipid-lowering effect, which, along with the antioxidant properties, points to consider feruloyl amides for further investigations in a therapeutic perspective.     

不对称芳基取代的方酰胺和异方酰胺的合成

Ｎ－芳基氮氧方酸的活性羟基能够被芳伯胺取代。利用这一特性，可在方酸四碳环上引入另一不同的芳胺基，即可获得不对称芳基取代的方酰胺或异方酰胺。以乙醇等为介质，芳伯胺与７种Ｎ－芳基氮方酸反应，制得２５个不对称的方酰胺和２４个不对称的异方酰胺。该合成方法优点突出，反应简便有效，通用性强。     

A Keggin-Type Tungstovanadate-Based Hybrid Compound: Synthesis,Crystal Structure,and Electrocatalytic Oxidation of Ascorbic Acid

Russian Journal of Coordination Chemistry - A new V-centered Keggin polyoxometalate-based inorganic-organic hybrid (HPpz)3[VW12O40] (I) (Ppz = piperazine) has been hydrothermal synthesized and...     

Oxidation of Thioamides to Amides with Tetrachloro- and Tetrabromoglycolurils

Russian Journal of Organic Chemistry - Tetrabromo- and tetrachloroglycolurils have been shown to act as good oxidants capable of converting thioamides to the corresponding amides. This approach...     

A Convenient One-Pot Synthesis and Nematicidal Activity of Nicotinic Acid Amides

Russian Journal of Organic Chemistry - Seven nicotinic acid amides were synthesized by condensation of nicotinic acid adsorbed on silica gel with different aromatic amines. The synthesized...     

Synthesis and Thermotropic Behavior of Simple New Glucolipid Amides

The coupling reaction of 3,4,6‐tri‐O‐acetyl‐α‐d‐glucopyranoside 2‐O‐lactone 1 (α‐CMGL) with two kinds of lipophilic amines, aminosteroids and fatty amines, efficiently yielded, after deprotection, the corresponding free α‐glucolipid amides. The latter family of compounds exhibited good thermal stability, allowing the higher homologs having longer linear fatty chains or saturated steroids to possess lamellar smectic A phases.     

生物碱Actinophyllic Acid三环中间体的不对称合成

以(S)-3-(2,2-二甲基-5-(3-甲基-1H-吲哚-2-基)-1,3-二氧杂环己烷-5-基)吡咯烷-2-酮为原料,经吡咯烷酮还原开环、串联的氢化脱保护/分子内还原胺化反应等关键步骤,合成了吲哚生物碱actinophyllic acid的A/B/C环手性中间体(S)-3-(2-(2-氯乙酰氨基)-2′,2′-二甲基-1,2,3,4,5,7-六氢螺[氮杂环辛烷并[4,3-b]吲哚-6,5′-[1,3]二氧杂环己烷]-5-基)-3-丙酮酸甲酯（9）; 9可在氧化条件下转化为A/B/G环中间体(S)-7-(2-(2-氯乙酰氨基)乙基)-2′,2′-二甲基-8-氧代-7,8-二氢-5-H-螺[环庚烯并[b]吲哚-6,5′-[1,3]二氧杂环己烷]-9-甲酸酯（10）。该合成路线涉及9个新化合物,其结构经¹H NMR,¹³C NMR, 2D NMR和LC-MS(ESI)表征。     

Synthesis,Quantification, and Characterization of Fatty Acid Amides from In Vitro and In Vivo Sources

Fatty acid amides are a diverse family of underappreciated, biologically occurring lipids. Herein, the methods for the chemical synthesis and subsequent characterization of specific members of the fatty acid amide family are described. The synthetically prepared fatty acid amides and those obtained commercially are used as standards for the characterization and quantification of the fatty acid amides produced by biological systems, a fatty acid amidome. The fatty acid amidomes from mouse N₁₈TG₂ cells, sheep choroid plexus cells, Drosophila melanogaster, Bombyx mori, Apis mellifera, and Tribolium castaneum are presented.     

Phase Transfer Catalyzed Synthesis of Amides and Esters of 2,4-Dichlorophenoxyacetic Acid

A convenient procedure is reported for the preparation of amides and esters via the reaction of 2,4-dichlorophenoxyacetyl chloride with amines or phenols under the condition of liquid-liquid phase transfer catalysis using polyethylene gtycol-600 as the catalyst. The products have been characterised on the basis of analytical and spectral (IR and H-NMR) data.