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
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
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
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 spectrophotomet...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
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.
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.
