By using 1-methyl-2-formyl-5 -Y-substituted pyrrole (4-nitrophenyl)hydrazones as a model for nitrogen-containing heterocyclic aromatic compounds, the emission wavelength [lambda(max(em))] values df their fluorescence ...By using 1-methyl-2-formyl-5 -Y-substituted pyrrole (4-nitrophenyl)hydrazones as a model for nitrogen-containing heterocyclic aromatic compounds, the emission wavelength [lambda(max(em))] values df their fluorescence spectra have been measured. Correlation results show that the Delta E-em values are mainly affected by polar effects, but spin-delocalizatin effects also exist.展开更多
4,5-Dibromo-1-methyl-2-trichloroacetylpyrrole Ⅰ, prepared by the reaction of 1-methyl-2-trichloroacetylpyrrole with Br2 in 98.6 % yield, was condensed with methyl L-2-amino-3- phenylpropanoate to afford methyl 2-（4,...4,5-Dibromo-1-methyl-2-trichloroacetylpyrrole Ⅰ, prepared by the reaction of 1-methyl-2-trichloroacetylpyrrole with Br2 in 98.6 % yield, was condensed with methyl L-2-amino-3- phenylpropanoate to afford methyl 2-（4,5-dibromo-1-methylpyrrole-2-carboxmido）-3-phenylpropanoate Ⅱ in 90.8% yield. Crystal data for Ⅰ： monoclinic system, space group P21/c with a = 8.595（3）, b = 10.900（4）, c = 12.321（5） ,A°,β = 92.292（7）°, V = 1153.4（8）A°^3, Dc = 2.213 g/cm^3, F（000） = 728, CTH4Br2Cl3NO, Mr = 384.28, λ = 0.71073 A°, μ（MoKa） = 7.688 mm^-1, Z = 4, R = 0.0338 and wR2 = 0.0840 for 1963 observed reflections with I 〉 2a（I）. Crystal data for Ⅱ： monoclinic system, space group P21 with a = 4.886（2）, b = 15.921（8）, c = 11.635（6） A°,β = 101.803（9）°, V = 885.9（7） A°^3, Dc = 1.665 g/cm^3, F（000） = 440, C16H16Br2N2O3, Mr = 444.13, λ = 0.71073 A°, μ（MoKa） = 4.590 mm^-1, Z = 2, R = 0.0335 and wR2 = 0.0837 for 3191 observed reflections with I 〉 2σ（I）. The crystal structure reveals that compound Ⅱ forms the one-dimensional chain structure via the intermolecular hydrogen bonds of N（2）-H…O（1）.展开更多
Mono-substituted heterocyclic ketene aminals are formed by the reaction of 1-methyl-2-methylthio-imidazoline with active methylene compounds containinq an acetyl or benzoyl group by the elimination of both a methylthi...Mono-substituted heterocyclic ketene aminals are formed by the reaction of 1-methyl-2-methylthio-imidazoline with active methylene compounds containinq an acetyl or benzoyl group by the elimination of both a methylthio and an acyl group.This is resulted by the secondary reactio of the produced methanethiol to attack the more active carbonyl group.展开更多
Sodium 3,5-bis(hydroxyimino)-1-methyl-2,4,6-trioxocyclohexanide C7H5N2NaO5 (I) has been isolated as the only product of the reaction of nitrosation of methylphloroglucinol. The structure of the titled compound has bee...Sodium 3,5-bis(hydroxyimino)-1-methyl-2,4,6-trioxocyclohexanide C7H5N2NaO5 (I) has been isolated as the only product of the reaction of nitrosation of methylphloroglucinol. The structure of the titled compound has been determined from single crystal X-ray diffraction data. The hydrated C7H5N2NaO52.5H2O crystallizes in the monoclinic space group C2/c, with a(?) 16.408(3);b(?) 12.446(3);c(?) 13.716(3);(o) 126.34(3). The planar organic anion exists in a triketo-dihydroxyimino form with the C–O and C–N distances from 1.220(2) to 1.271(2)?? and from 1.292(2) to 1.293?? respectively. In the IR spectrum of I, the sharp absorption band occurred at 1681 cm-1 due to C=O stretching indicating the strong H-interactions. The correlations of theoretical (DFT-B3LYP/aug-cc-pVDZ) and experimental UV-vis absorption spectra in neutral and alkaline ethanolic solutions showed the existence of hydroxyimino-nitroso tautomerism while ionization of I.展开更多
建立了一种在温和条件下,用可见光催化合成一系列3,4-二氢异喹啉-1(2H)-酮及其衍生物的方法。该方法在室温条件下,以2-烯丙基-N-甲氧基苯甲酰胺为模板底物,以碘化钾作为光催化剂,25 W 460 nm的蓝色LED灯照射下,合成一系列3,4-二氢异喹啉...建立了一种在温和条件下,用可见光催化合成一系列3,4-二氢异喹啉-1(2H)-酮及其衍生物的方法。该方法在室温条件下,以2-烯丙基-N-甲氧基苯甲酰胺为模板底物,以碘化钾作为光催化剂,25 W 460 nm的蓝色LED灯照射下,合成一系列3,4-二氢异喹啉-1(2H)-酮衍生物,最高产率可达到83%。该合成路径具有底物适用范围广、经济实用等特点,为3,4-二氢异喹啉-1(2H)-酮衍生物合成提供了一种经济简便的方法。展开更多
目的观察火针联合董氏奇穴针刺治疗肩袖损伤的临床疗效及对关节功能及血清前列腺素E_(2)(prostaglandin E_(2),PGE_(2))和转化生长因子-β1(transforming growth factor-β1,TGF-β1)的影响。方法将100例肩袖损伤患者随机分为对照组(50...目的观察火针联合董氏奇穴针刺治疗肩袖损伤的临床疗效及对关节功能及血清前列腺素E_(2)(prostaglandin E_(2),PGE_(2))和转化生长因子-β1(transforming growth factor-β1,TGF-β1)的影响。方法将100例肩袖损伤患者随机分为对照组(50例)和观察组(50例)。对照组予以电针联合董氏奇穴针刺治疗,观察组予以火针联合董氏奇穴针刺治疗。检测视觉模拟量表(visual analog scale,VAS)和美国加利福尼亚大学洛杉矶分校(University of California,Los Angeles,UCLA)肩关节评分、肩关节活动度(range of motion,ROM)及血清PGE_(2)和TGF-β1水平。结果观察组总有效率高于对照组(P<0.05)。治疗后及4周随访时,两组VAS评分及血清PGE_(2)和TGF-β1水平均低于治疗前(P<0.05),且观察组均低于对照组(P<0.05);两组UCLA肩关节评分和肩关节ROM均高于治疗前(P<0.05),且观察组均高于对照组(P<0.05)。4周随访时,两组VAS评分、UCLA肩关节评分、肩关节ROM及血清PGE_(2)和TGF-β1水平与治疗后比较差异无统计系意义(P>0.05)。治疗后血清PGE_(2)、TGF-β1水平与VAS评分呈正相关,与UCLA肩关节评分呈负相关。结论火针和电针联合董氏奇穴针刺治疗肩袖损伤均可缓解疼痛、改善肩关节功能,但火针优于电针,其机制可能与降低血清PGE_(2)和TGF-β1水平有关。展开更多
文摘By using 1-methyl-2-formyl-5 -Y-substituted pyrrole (4-nitrophenyl)hydrazones as a model for nitrogen-containing heterocyclic aromatic compounds, the emission wavelength [lambda(max(em))] values df their fluorescence spectra have been measured. Correlation results show that the Delta E-em values are mainly affected by polar effects, but spin-delocalizatin effects also exist.
基金The project was supported by the National 863 Program of China (No. 2004AA628030), and Natural Science Foundation of Guangdong Province (No. 31920)
文摘4,5-Dibromo-1-methyl-2-trichloroacetylpyrrole Ⅰ, prepared by the reaction of 1-methyl-2-trichloroacetylpyrrole with Br2 in 98.6 % yield, was condensed with methyl L-2-amino-3- phenylpropanoate to afford methyl 2-（4,5-dibromo-1-methylpyrrole-2-carboxmido）-3-phenylpropanoate Ⅱ in 90.8% yield. Crystal data for Ⅰ： monoclinic system, space group P21/c with a = 8.595（3）, b = 10.900（4）, c = 12.321（5） ,A°,β = 92.292（7）°, V = 1153.4（8）A°^3, Dc = 2.213 g/cm^3, F（000） = 728, CTH4Br2Cl3NO, Mr = 384.28, λ = 0.71073 A°, μ（MoKa） = 7.688 mm^-1, Z = 4, R = 0.0338 and wR2 = 0.0840 for 1963 observed reflections with I 〉 2a（I）. Crystal data for Ⅱ： monoclinic system, space group P21 with a = 4.886（2）, b = 15.921（8）, c = 11.635（6） A°,β = 101.803（9）°, V = 885.9（7） A°^3, Dc = 1.665 g/cm^3, F（000） = 440, C16H16Br2N2O3, Mr = 444.13, λ = 0.71073 A°, μ（MoKa） = 4.590 mm^-1, Z = 2, R = 0.0335 and wR2 = 0.0837 for 3191 observed reflections with I 〉 2σ（I）. The crystal structure reveals that compound Ⅱ forms the one-dimensional chain structure via the intermolecular hydrogen bonds of N（2）-H…O（1）.
文摘Mono-substituted heterocyclic ketene aminals are formed by the reaction of 1-methyl-2-methylthio-imidazoline with active methylene compounds containinq an acetyl or benzoyl group by the elimination of both a methylthio and an acyl group.This is resulted by the secondary reactio of the produced methanethiol to attack the more active carbonyl group.
文摘Sodium 3,5-bis(hydroxyimino)-1-methyl-2,4,6-trioxocyclohexanide C7H5N2NaO5 (I) has been isolated as the only product of the reaction of nitrosation of methylphloroglucinol. The structure of the titled compound has been determined from single crystal X-ray diffraction data. The hydrated C7H5N2NaO52.5H2O crystallizes in the monoclinic space group C2/c, with a(?) 16.408(3);b(?) 12.446(3);c(?) 13.716(3);(o) 126.34(3). The planar organic anion exists in a triketo-dihydroxyimino form with the C–O and C–N distances from 1.220(2) to 1.271(2)?? and from 1.292(2) to 1.293?? respectively. In the IR spectrum of I, the sharp absorption band occurred at 1681 cm-1 due to C=O stretching indicating the strong H-interactions. The correlations of theoretical (DFT-B3LYP/aug-cc-pVDZ) and experimental UV-vis absorption spectra in neutral and alkaline ethanolic solutions showed the existence of hydroxyimino-nitroso tautomerism while ionization of I.
文摘建立了一种在温和条件下,用可见光催化合成一系列3,4-二氢异喹啉-1(2H)-酮及其衍生物的方法。该方法在室温条件下,以2-烯丙基-N-甲氧基苯甲酰胺为模板底物,以碘化钾作为光催化剂,25 W 460 nm的蓝色LED灯照射下,合成一系列3,4-二氢异喹啉-1(2H)-酮衍生物,最高产率可达到83%。该合成路径具有底物适用范围广、经济实用等特点,为3,4-二氢异喹啉-1(2H)-酮衍生物合成提供了一种经济简便的方法。
文摘目的观察火针联合董氏奇穴针刺治疗肩袖损伤的临床疗效及对关节功能及血清前列腺素E_(2)(prostaglandin E_(2),PGE_(2))和转化生长因子-β1(transforming growth factor-β1,TGF-β1)的影响。方法将100例肩袖损伤患者随机分为对照组(50例)和观察组(50例)。对照组予以电针联合董氏奇穴针刺治疗,观察组予以火针联合董氏奇穴针刺治疗。检测视觉模拟量表(visual analog scale,VAS)和美国加利福尼亚大学洛杉矶分校(University of California,Los Angeles,UCLA)肩关节评分、肩关节活动度(range of motion,ROM)及血清PGE_(2)和TGF-β1水平。结果观察组总有效率高于对照组(P<0.05)。治疗后及4周随访时,两组VAS评分及血清PGE_(2)和TGF-β1水平均低于治疗前(P<0.05),且观察组均低于对照组(P<0.05);两组UCLA肩关节评分和肩关节ROM均高于治疗前(P<0.05),且观察组均高于对照组(P<0.05)。4周随访时,两组VAS评分、UCLA肩关节评分、肩关节ROM及血清PGE_(2)和TGF-β1水平与治疗后比较差异无统计系意义(P>0.05)。治疗后血清PGE_(2)、TGF-β1水平与VAS评分呈正相关,与UCLA肩关节评分呈负相关。结论火针和电针联合董氏奇穴针刺治疗肩袖损伤均可缓解疼痛、改善肩关节功能,但火针优于电针,其机制可能与降低血清PGE_(2)和TGF-β1水平有关。
