The novel title compound（Z）-N-（4-bromo-5-ethoxy-3,5-dimethylfuran-2（5H）-yli-dene）-4-methylbenzenesulfonamide 1（C15H18BrNO4S） has been unexpectedly synthesized by the aminohalogenation reaction of ethyl 2-methy...The novel title compound（Z）-N-（4-bromo-5-ethoxy-3,5-dimethylfuran-2（5H）-yli-dene）-4-methylbenzenesulfonamide 1（C15H18BrNO4S） has been unexpectedly synthesized by the aminohalogenation reaction of ethyl 2-methylpenta-2,3-dienoate with TsNBr2,and characterized by mp,IR,1H NMR,EIMS,ESIHRMS and single-crystal X-ray diffraction.It crystallizes in mono-clinic,space group P21/c with a = 11.714（5）,b = 14.106（5）,c = 10.402（4） ,β = 97.298（8）°,V = 1704.9（12） 3,Mr = 388.27,Z = 4,Dc = 1.513 g/cm3,μ（MoKα） = 2.549 mm-1,F（000） = 792,the final R = 0.033 and wR = 0.062 for 3098 observed reflections（Ⅰ 〉 2σ（Ⅰ））.展开更多
Due to acidic solutions aggressiveness, corrosion inhibitors use is considered to be one the most practical methods to delay metals dissolution in the said solutions. In this study benzimidazolyl derivative namely 2-c...Due to acidic solutions aggressiveness, corrosion inhibitors use is considered to be one the most practical methods to delay metals dissolution in the said solutions. In this study benzimidazolyl derivative namely 2-cyanochalcones 2-(5-nitro-1,3-dihydrobenzimidazol-2-ylidene)-3-oxo-3-(2-oxo-2H-chromen-3-yl) propanenitrile which was synthesized was then applied as a corrosion inhibitor for copper in 1 M HNO<sub>3</sub> solution. The inhibition action of this molecule was evaluated by gravimetric and density functional theory (DFT) methods. It was found experimentally that this compound has a better inhibition performance and its adsorption on copper surface follows Langmuir adsorption isotherm. This adsorption evolves with temperature and inhibitor concentration, it is endothermic and occurs spontaneously with an increase in disorder. Corrosion kinetic parameters analysis supported by Adejo-Ekwenchi model revealed the existence of both physisorption and chemisorption. DFT calculations related that compound adsorption on copper surface is due to its electron donating and accepting capacity. The reactive regions specifying the electrophilic and nucleophilic attack sites were analyzed using Fukui and dual descriptor functions. Experimental results obtained were compared with the theoretical findings.展开更多
Synthesis of the title compound was carried out by base-catalyzed cyclization of 1-pivaloyl-3-(2-chloro-4-nitrophenyl) thiourea with α-bromoacetone produced in situ. The structure was confirmed by the spectroscopic a...Synthesis of the title compound was carried out by base-catalyzed cyclization of 1-pivaloyl-3-(2-chloro-4-nitrophenyl) thiourea with α-bromoacetone produced in situ. The structure was confirmed by the spectroscopic and elemental analysis and single crystal X-ray diffraction data. It crystallizes in the triclinic space group P-1 with unit cell dime sions a = 8.7137(10), b = 10.2010(14), c = 10.6593(13), α = 62.671(9), β = 82.701(10), γ = 79.762(10), V = 827.21(8) ?3, Z = 2.展开更多
目的研究在没有对照品的情况下鉴定检材中1-(4-氟苯基)-2-(N-吡咯烷基)-1-戊酮[1-(4-fluorophenyl)-2-(1-pyrrolidinyl)pentan-1-one,4-F-α-PVP]类似物1-(4-氟-3甲基苯基)-2-(N-吡咯烷基)-1-戊酮[1-(4-fluoro-3-methyl phenyl)-2-(1-py...目的研究在没有对照品的情况下鉴定检材中1-(4-氟苯基)-2-(N-吡咯烷基)-1-戊酮[1-(4-fluorophenyl)-2-(1-pyrrolidinyl)pentan-1-one,4-F-α-PVP]类似物1-(4-氟-3甲基苯基)-2-(N-吡咯烷基)-1-戊酮[1-(4-fluoro-3-methyl phenyl)-2-(1-pyrrolidinyl)pentan-1-one,4-F-3-Methyl-α-PVP]盐酸盐的方法。方法综合利用直接进样电子电离-质谱(electron ionization-mass spectrometry,EI-MS)、GCMS、电喷雾离子化-高分辨质谱(electrospray ionization-high resolution mass spectrometry,ESI-HRMS)、超高效液相色谱-高分辨串联质谱(ultra-high performance liquid chromatography-high resolution tandem mass spectrometry,UPLC-HRMS/MS)、核磁共振(nuclear magnetic resonance,NMR)、离子色谱和傅里叶变换红外光谱法(Fourier transform infrared spectroscopy,FTIR),实现对检材中未知化合物的结构解析与表征,并对该化合物在EI-MS和UPLC-HRMS/MS两种质谱分析方式下生成碎片离子的裂解机制进行推导。结果通过对检材中化合物的直接进样EI-MS、GC-MS、ESI-HRMS和UPLC-HRMS/MS分析,推断出未知化合物为4-F-α-PVP的结构类似物,可能苯环中多了1个甲基。根据核磁共振氢谱(1H-nuclear magnetic reso⁃nance,1 H-NMR)、核磁共振碳谱(13C-nuclear magnetic resonance,13C-NMR)等分析结果,进一步证明了甲基的位置在苯环的3-位。由于1H-NMR分析中实际氢的个数比4-F-3-Methyl-α-PVP中性分子多1个,推断该化合物以盐形式存在。离子色谱法分析结果表明该化合物含氯离子(含量11.14%~11.16%),结合FTIR对主要官能团信息的结构分析,最终确定该未知化合物为4-F-3-Methyl-α-PVP盐酸盐。结论建立了综合利用EI-MS、GC-MS、ESI-HRMS、UPLC-HRMS/MS、NMR、离子色谱和FTIR鉴定检材中4-F-3-Methyl-α-PVP盐酸盐的方法,将有助于法庭科学实验室在案件中鉴定该物质或其他具有类似结构的化合物。展开更多
文摘The novel title compound（Z）-N-（4-bromo-5-ethoxy-3,5-dimethylfuran-2（5H）-yli-dene）-4-methylbenzenesulfonamide 1（C15H18BrNO4S） has been unexpectedly synthesized by the aminohalogenation reaction of ethyl 2-methylpenta-2,3-dienoate with TsNBr2,and characterized by mp,IR,1H NMR,EIMS,ESIHRMS and single-crystal X-ray diffraction.It crystallizes in mono-clinic,space group P21/c with a = 11.714（5）,b = 14.106（5）,c = 10.402（4） ,β = 97.298（8）°,V = 1704.9（12） 3,Mr = 388.27,Z = 4,Dc = 1.513 g/cm3,μ（MoKα） = 2.549 mm-1,F（000） = 792,the final R = 0.033 and wR = 0.062 for 3098 observed reflections（Ⅰ 〉 2σ（Ⅰ））.
文摘Due to acidic solutions aggressiveness, corrosion inhibitors use is considered to be one the most practical methods to delay metals dissolution in the said solutions. In this study benzimidazolyl derivative namely 2-cyanochalcones 2-(5-nitro-1,3-dihydrobenzimidazol-2-ylidene)-3-oxo-3-(2-oxo-2H-chromen-3-yl) propanenitrile which was synthesized was then applied as a corrosion inhibitor for copper in 1 M HNO<sub>3</sub> solution. The inhibition action of this molecule was evaluated by gravimetric and density functional theory (DFT) methods. It was found experimentally that this compound has a better inhibition performance and its adsorption on copper surface follows Langmuir adsorption isotherm. This adsorption evolves with temperature and inhibitor concentration, it is endothermic and occurs spontaneously with an increase in disorder. Corrosion kinetic parameters analysis supported by Adejo-Ekwenchi model revealed the existence of both physisorption and chemisorption. DFT calculations related that compound adsorption on copper surface is due to its electron donating and accepting capacity. The reactive regions specifying the electrophilic and nucleophilic attack sites were analyzed using Fukui and dual descriptor functions. Experimental results obtained were compared with the theoretical findings.
文摘Synthesis of the title compound was carried out by base-catalyzed cyclization of 1-pivaloyl-3-(2-chloro-4-nitrophenyl) thiourea with α-bromoacetone produced in situ. The structure was confirmed by the spectroscopic and elemental analysis and single crystal X-ray diffraction data. It crystallizes in the triclinic space group P-1 with unit cell dime sions a = 8.7137(10), b = 10.2010(14), c = 10.6593(13), α = 62.671(9), β = 82.701(10), γ = 79.762(10), V = 827.21(8) ?3, Z = 2.
文摘目的研究在没有对照品的情况下鉴定检材中1-(4-氟苯基)-2-(N-吡咯烷基)-1-戊酮[1-(4-fluorophenyl)-2-(1-pyrrolidinyl)pentan-1-one,4-F-α-PVP]类似物1-(4-氟-3甲基苯基)-2-(N-吡咯烷基)-1-戊酮[1-(4-fluoro-3-methyl phenyl)-2-(1-pyrrolidinyl)pentan-1-one,4-F-3-Methyl-α-PVP]盐酸盐的方法。方法综合利用直接进样电子电离-质谱(electron ionization-mass spectrometry,EI-MS)、GCMS、电喷雾离子化-高分辨质谱(electrospray ionization-high resolution mass spectrometry,ESI-HRMS)、超高效液相色谱-高分辨串联质谱(ultra-high performance liquid chromatography-high resolution tandem mass spectrometry,UPLC-HRMS/MS)、核磁共振(nuclear magnetic resonance,NMR)、离子色谱和傅里叶变换红外光谱法(Fourier transform infrared spectroscopy,FTIR),实现对检材中未知化合物的结构解析与表征,并对该化合物在EI-MS和UPLC-HRMS/MS两种质谱分析方式下生成碎片离子的裂解机制进行推导。结果通过对检材中化合物的直接进样EI-MS、GC-MS、ESI-HRMS和UPLC-HRMS/MS分析,推断出未知化合物为4-F-α-PVP的结构类似物,可能苯环中多了1个甲基。根据核磁共振氢谱(1H-nuclear magnetic reso⁃nance,1 H-NMR)、核磁共振碳谱(13C-nuclear magnetic resonance,13C-NMR)等分析结果,进一步证明了甲基的位置在苯环的3-位。由于1H-NMR分析中实际氢的个数比4-F-3-Methyl-α-PVP中性分子多1个,推断该化合物以盐形式存在。离子色谱法分析结果表明该化合物含氯离子(含量11.14%~11.16%),结合FTIR对主要官能团信息的结构分析,最终确定该未知化合物为4-F-3-Methyl-α-PVP盐酸盐。结论建立了综合利用EI-MS、GC-MS、ESI-HRMS、UPLC-HRMS/MS、NMR、离子色谱和FTIR鉴定检材中4-F-3-Methyl-α-PVP盐酸盐的方法,将有助于法庭科学实验室在案件中鉴定该物质或其他具有类似结构的化合物。
