Five DTPA bis(amide)s have been synthesized and characterized by means of 1 H NMR , FT IR and elemental analyses. The stability constants of their Gd 3+ complexes have been measured using a simple spec...Five DTPA bis(amide)s have been synthesized and characterized by means of 1 H NMR , FT IR and elemental analyses. The stability constants of their Gd 3+ complexes have been measured using a simple spectrophotometric method. The results show that the complexing properties of the ligands in comparison with those of DTPA are affected by converting two carboxyl groups to amide groups. The relaxation studies have shown that the relaxivity of the chelates is similar to that of Gd DTPA, indicating that in solution all the chelates have one water molecule directly coordinated to the metal ion. Only one water molecule in inner coordination sphere suggests the coordination of the carboxamide oxygen to gadolinium ion, which agrees with the FT IR results.展开更多
A series of novel aromatic poly ( amide imide)s containing phthalazinone moieties were prepared from 2-(4-aminophenyl)-4-[3-methyl-4-(4-aminophenoxy)-2,3-phthalazinone-1], a novel diamine 1 with four diimide-dicarboxy...A series of novel aromatic poly ( amide imide)s containing phthalazinone moieties were prepared from 2-(4-aminophenyl)-4-[3-methyl-4-(4-aminophenoxy)-2,3-phthalazinone-1], a novel diamine 1 with four diimide-dicarboxylic acids by Yamazaki phosphorylation method with the inherent viscosity of 0.36~0.65 dL/g. These polymers had high glass transition temperatures above 300C and they lost 10% weight between 426~475C in N2. The structure of diamine 1 and the polymers was confirmed by IR, 1H NMR and MS. The obtained polymers were readily soluble in polar solvents such as NMP, m-cresol etc. and easily cast into tough, flexible films. The X-ray indicated that they are all amorphous.展开更多
An efficient and simple method for the synthesis of new chiral aromatic amide molecular tweezers by irradiation with microwave under solvent-free conditions has been developed. Its main advantages are short reaction t...An efficient and simple method for the synthesis of new chiral aromatic amide molecular tweezers by irradiation with microwave under solvent-free conditions has been developed. Its main advantages are short reaction times, good conversions and the environmentally friendly nature of the process.展开更多
Herein,we report a condition-controlled divergent synthesis of spiro indene-2,1'-isoindolinones and spiro isochroman-3,1'-isoindolinones through cobalt-catalyzed formal[4+1]and[4+1+1]spirocyclization of aromat...Herein,we report a condition-controlled divergent synthesis of spiro indene-2,1'-isoindolinones and spiro isochroman-3,1'-isoindolinones through cobalt-catalyzed formal[4+1]and[4+1+1]spirocyclization of aromatic amides with 2-diazo-1H-indene-1,3(2H)-dione.When the reaction is carried out under air in ethyl acetate,spiro indene-2,1'-isoindolinones are formed through Co(II)-catalyzed C—H/N—H[4+1]spirocyclization.When the reaction is run under O2 in CH3CN,on the other hand,spiro isochroman-3,1'-isoindolinones are generated through Baeyer-Villiger oxidation of the in situ formed spiro indene-2,1'-isoindolinones with O2 as a cheaper and environmental-friendly oxygen source.In general,these protocols have advantages such as using non-precious and earth-abundant metal catalyst,no extra additive,high efficiency and regioselectivity.A gram-scale synthesis and the removal of the directing group further highlight its utility.展开更多
In the synthesis of l-phenyl-5-substituted amino-4-pyrazole N-alkyl amide, it was found for the first time that one of the two aromatic amido groups in the molecule of 1-phenyl-5-benzoyl amino-4-pyrazole N-alkyl amide...In the synthesis of l-phenyl-5-substituted amino-4-pyrazole N-alkyl amide, it was found for the first time that one of the two aromatic amido groups in the molecule of 1-phenyl-5-benzoyl amino-4-pyrazole N-alkyl amide was reduced selectively by LiAlH_4. new conclusion was drawn after several experiments have been done that ortho-amino(or substituted amino)aryl amide or the aryl amide with its ortho substituent which can be reduced into an amino group(or substituted amino group)can not be reduced by LiAlH_4. It was further rationalized by quantum chemical calculation.展开更多
A new wo-armed?acyclic diamide Ia 2, 6-bis(1-ethanecarbozamido-2-amino)pyridine, and a new series of aromatic aldehyde schiff bases containing pyridine ring and amide bridge, IIa-f, were prepared. The compounds were...A new wo-armed?acyclic diamide Ia 2, 6-bis(1-ethanecarbozamido-2-amino)pyridine, and a new series of aromatic aldehyde schiff bases containing pyridine ring and amide bridge, IIa-f, were prepared. The compounds were characterized by elemental analysis, IR, 1HNMR and MS. The bioactivity half inhibitory concentration C1/2 is given.展开更多
Two benzene/2,2＇-bipyridine-alternately incorporated amide polymers have been prepared, which are driven by hydrophobicity to form two different helical conformations. Both helices exhibit twist sense bias in water i...Two benzene/2,2＇-bipyridine-alternately incorporated amide polymers have been prepared, which are driven by hydrophobicity to form two different helical conformations. Both helices exhibit twist sense bias in water induced by chiral valine side chains and the coordination of the 2,2＇-bipyridine unit to the Ni2＋ ions.展开更多
Intramolecular N H···X (X=F, Cl, Br, and Ⅰ) hydrogen bonding patterns of aromatic amides in the solid state are summarized. It is revealed that the key for the formation of this kind of weak intramolec...Intramolecular N H···X (X=F, Cl, Br, and Ⅰ) hydrogen bonding patterns of aromatic amides in the solid state are summarized. It is revealed that the key for the formation of this kind of weak intramolecular hydrogen bonding in X-ray crystal structures is to suppress the competition of strong intermolecular N H···O C hydrogen bonding of the amide unit. For amides with identical backbones, the bonding capacity of halogen atoms as hydrogen bonding acceptors is in the order of F>Cl>Br>I, which is in accordance with their electronegativity strength. Generally, the five-membered hydrogen bonding is easier to form than the six-membered one.展开更多
Ⅰ. INTRODUCTION Recently, we demonstrated that active acylamide of benzotriazole (HBT) has the ability of selective N-acylation with aminoalcohols except the N-acylation
polyamide type has been studied under both electron and optical microscopes. Membranes of the aromatic polyamide type are prepared from corresponding polymeric solutions in N, N-dimethyl acetamide. The casting solutio...polyamide type has been studied under both electron and optical microscopes. Membranes of the aromatic polyamide type are prepared from corresponding polymeric solutions in N, N-dimethyl acetamide. The casting solution was spread with a glass knife over a glass plate to a definite thickness and was heated on a展开更多
The n-acetoacetyl aromatic amide of complexes of copper (Ⅱ)and their ice nucleation has not yet been published. The reactants of the title complexes are cheap and the synthetic method is simple. A mixture of methanol...The n-acetoacetyl aromatic amide of complexes of copper (Ⅱ)and their ice nucleation has not yet been published. The reactants of the title complexes are cheap and the synthetic method is simple. A mixture of methanol so-展开更多
The receptor derived from the diethoxycarbonyl glycoluril was synthesized and characterized by IR,^(1)H NMR,MS techniques and X-ray single crystal analysis.Single crystal X-ray diffraction reveals that the receptor re...The receptor derived from the diethoxycarbonyl glycoluril was synthesized and characterized by IR,^(1)H NMR,MS techniques and X-ray single crystal analysis.Single crystal X-ray diffraction reveals that the receptor remains monomeric because of its bulky t-Bu groups on the side walls.Its unique binding properties for aromatic amides were studied through ^(1)H NMR and IR techniques.展开更多
A series organosoluble and heterocyclic poly（ether-amide）s （PEA）s were synthesized from a new diamine containing pyridine moiety and four aliphatic-aromatic dicarboxylic acids by direct polycondensation reactions....A series organosoluble and heterocyclic poly（ether-amide）s （PEA）s were synthesized from a new diamine containing pyridine moiety and four aliphatic-aromatic dicarboxylic acids by direct polycondensation reactions. Dicarboxilic acids 4a-4d containing ether groups were synthesized in two step reactions. At first, dialdehydes 3a-3d were synthesized from four dibromo alkanes la-ld and 4-hydroxybenzaldehyde 2, then dicarboxilic acids 4a-4d were synthesized from dialdehydes 3a-3d and malonic acid in a solvent free reaction. On the other hand, the new diamine 8 containing pyridine ring was synthesized in two step reactions. The structures of synthesized monomers and polymers were proven by FTIR, NMR spectroscopy and elemental analysis. Also all of the above polymers were fully characterized by inherent viscosity, solubility tests, gel permeation chromatography （GPC）, differential scanning calorimetry （DSC） and thermogravimetric analysis （TGA）. The resulted PEAs have shown good inherent viscosities, solubility and thermal properties.展开更多
采用硅胶柱色谱和半制备反相高效液相色谱分离方法,对南海海洋放线菌Streptomyces lusitanus SCSIOLR32的次级代谢产物进行了研究,分离得到四个酰胺类化合物,经MS1、H和13 C NMR波谱分析鉴定为二甲基甲苯2,4-二氨基甲酸甲酯(1),甲苯2,4...采用硅胶柱色谱和半制备反相高效液相色谱分离方法,对南海海洋放线菌Streptomyces lusitanus SCSIOLR32的次级代谢产物进行了研究,分离得到四个酰胺类化合物,经MS1、H和13 C NMR波谱分析鉴定为二甲基甲苯2,4-二氨基甲酸甲酯(1),甲苯2,4-二氨基甲酸乙酯(2),甲苯2,6-二氨基甲酸甲酯(3)和甲苯2,6-二氨基甲酸乙酯(4)。运用X-单晶衍射确定了1的结构式。其中化合物2和4是首次从自然界中分离得到。采用16S分子生物学方法鉴定该菌株为链霉菌属放线菌。展开更多
文摘Five DTPA bis(amide)s have been synthesized and characterized by means of 1 H NMR , FT IR and elemental analyses. The stability constants of their Gd 3+ complexes have been measured using a simple spectrophotometric method. The results show that the complexing properties of the ligands in comparison with those of DTPA are affected by converting two carboxyl groups to amide groups. The relaxation studies have shown that the relaxivity of the chelates is similar to that of Gd DTPA, indicating that in solution all the chelates have one water molecule directly coordinated to the metal ion. Only one water molecule in inner coordination sphere suggests the coordination of the carboxamide oxygen to gadolinium ion, which agrees with the FT IR results.
文摘A series of novel aromatic poly ( amide imide)s containing phthalazinone moieties were prepared from 2-(4-aminophenyl)-4-[3-methyl-4-(4-aminophenoxy)-2,3-phthalazinone-1], a novel diamine 1 with four diimide-dicarboxylic acids by Yamazaki phosphorylation method with the inherent viscosity of 0.36~0.65 dL/g. These polymers had high glass transition temperatures above 300C and they lost 10% weight between 426~475C in N2. The structure of diamine 1 and the polymers was confirmed by IR, 1H NMR and MS. The obtained polymers were readily soluble in polar solvents such as NMP, m-cresol etc. and easily cast into tough, flexible films. The X-ray indicated that they are all amorphous.
基金supported by the Doctors Innovation Foundation of Southwest University for Nationalities(No.08NBS002).
文摘An efficient and simple method for the synthesis of new chiral aromatic amide molecular tweezers by irradiation with microwave under solvent-free conditions has been developed. Its main advantages are short reaction times, good conversions and the environmentally friendly nature of the process.
基金the National Natural Science Foundation of China(22101075,U2004189)Central Plains Science and Technology Innovation Leader Project(224200510009)+1 种基金Postdoctoral Research Grant in Henan Province(202103085)Henan Key Laboratory of Organic Functional Molecules and Drug Innovation,and 111 Project(D17007)for financial support.
文摘Herein,we report a condition-controlled divergent synthesis of spiro indene-2,1'-isoindolinones and spiro isochroman-3,1'-isoindolinones through cobalt-catalyzed formal[4+1]and[4+1+1]spirocyclization of aromatic amides with 2-diazo-1H-indene-1,3(2H)-dione.When the reaction is carried out under air in ethyl acetate,spiro indene-2,1'-isoindolinones are formed through Co(II)-catalyzed C—H/N—H[4+1]spirocyclization.When the reaction is run under O2 in CH3CN,on the other hand,spiro isochroman-3,1'-isoindolinones are generated through Baeyer-Villiger oxidation of the in situ formed spiro indene-2,1'-isoindolinones with O2 as a cheaper and environmental-friendly oxygen source.In general,these protocols have advantages such as using non-precious and earth-abundant metal catalyst,no extra additive,high efficiency and regioselectivity.A gram-scale synthesis and the removal of the directing group further highlight its utility.
基金Project supported by National Natural Science Foundation of China.
文摘In the synthesis of l-phenyl-5-substituted amino-4-pyrazole N-alkyl amide, it was found for the first time that one of the two aromatic amido groups in the molecule of 1-phenyl-5-benzoyl amino-4-pyrazole N-alkyl amide was reduced selectively by LiAlH_4. new conclusion was drawn after several experiments have been done that ortho-amino(or substituted amino)aryl amide or the aryl amide with its ortho substituent which can be reduced into an amino group(or substituted amino group)can not be reduced by LiAlH_4. It was further rationalized by quantum chemical calculation.
文摘A new wo-armed?acyclic diamide Ia 2, 6-bis(1-ethanecarbozamido-2-amino)pyridine, and a new series of aromatic aldehyde schiff bases containing pyridine ring and amide bridge, IIa-f, were prepared. The compounds were characterized by elemental analysis, IR, 1HNMR and MS. The bioactivity half inhibitory concentration C1/2 is given.
基金the Science and Technology Commission of Shanghai Munic- ipality （No. 13M1400200）, the Ministry of Science and Technology （No. 2013CB834501） and the Ministry of Education （Research Fund for the Doctoral Program） of China, and the National Science Foundation of China （Nos. 21432004 and 21272042）.
文摘Two benzene/2,2＇-bipyridine-alternately incorporated amide polymers have been prepared, which are driven by hydrophobicity to form two different helical conformations. Both helices exhibit twist sense bias in water induced by chiral valine side chains and the coordination of the 2,2＇-bipyridine unit to the Ni2＋ ions.
基金the National Natural Science Foundation of China (21172042and 20974118)the Ministry of Education of China (IR1117) for financial support
文摘Intramolecular N H···X (X=F, Cl, Br, and Ⅰ) hydrogen bonding patterns of aromatic amides in the solid state are summarized. It is revealed that the key for the formation of this kind of weak intramolecular hydrogen bonding in X-ray crystal structures is to suppress the competition of strong intermolecular N H···O C hydrogen bonding of the amide unit. For amides with identical backbones, the bonding capacity of halogen atoms as hydrogen bonding acceptors is in the order of F>Cl>Br>I, which is in accordance with their electronegativity strength. Generally, the five-membered hydrogen bonding is easier to form than the six-membered one.
文摘Ⅰ. INTRODUCTION Recently, we demonstrated that active acylamide of benzotriazole (HBT) has the ability of selective N-acylation with aminoalcohols except the N-acylation
文摘polyamide type has been studied under both electron and optical microscopes. Membranes of the aromatic polyamide type are prepared from corresponding polymeric solutions in N, N-dimethyl acetamide. The casting solution was spread with a glass knife over a glass plate to a definite thickness and was heated on a
文摘The n-acetoacetyl aromatic amide of complexes of copper (Ⅱ)and their ice nucleation has not yet been published. The reactants of the title complexes are cheap and the synthetic method is simple. A mixture of methanol so-
基金This work was supported by the Hubei University of Technology,Science and Technology Department of Hubei Province(No.ZRY0981)the National Natural Science Foundation of China(No.21272086).
文摘The receptor derived from the diethoxycarbonyl glycoluril was synthesized and characterized by IR,^(1)H NMR,MS techniques and X-ray single crystal analysis.Single crystal X-ray diffraction reveals that the receptor remains monomeric because of its bulky t-Bu groups on the side walls.Its unique binding properties for aromatic amides were studied through ^(1)H NMR and IR techniques.
文摘A series organosoluble and heterocyclic poly（ether-amide）s （PEA）s were synthesized from a new diamine containing pyridine moiety and four aliphatic-aromatic dicarboxylic acids by direct polycondensation reactions. Dicarboxilic acids 4a-4d containing ether groups were synthesized in two step reactions. At first, dialdehydes 3a-3d were synthesized from four dibromo alkanes la-ld and 4-hydroxybenzaldehyde 2, then dicarboxilic acids 4a-4d were synthesized from dialdehydes 3a-3d and malonic acid in a solvent free reaction. On the other hand, the new diamine 8 containing pyridine ring was synthesized in two step reactions. The structures of synthesized monomers and polymers were proven by FTIR, NMR spectroscopy and elemental analysis. Also all of the above polymers were fully characterized by inherent viscosity, solubility tests, gel permeation chromatography （GPC）, differential scanning calorimetry （DSC） and thermogravimetric analysis （TGA）. The resulted PEAs have shown good inherent viscosities, solubility and thermal properties.
文摘采用硅胶柱色谱和半制备反相高效液相色谱分离方法,对南海海洋放线菌Streptomyces lusitanus SCSIOLR32的次级代谢产物进行了研究,分离得到四个酰胺类化合物,经MS1、H和13 C NMR波谱分析鉴定为二甲基甲苯2,4-二氨基甲酸甲酯(1),甲苯2,4-二氨基甲酸乙酯(2),甲苯2,6-二氨基甲酸甲酯(3)和甲苯2,6-二氨基甲酸乙酯(4)。运用X-单晶衍射确定了1的结构式。其中化合物2和4是首次从自然界中分离得到。采用16S分子生物学方法鉴定该菌株为链霉菌属放线菌。
