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联苯吡菌胺关键中间体3′,4′-二氯-5-氟-1,1′-联苯-2-胺的合成
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作者 黄晓瑛 尚宇 +2 位作者 王威 王列平 毛明珍 《世界农药》 CAS 2024年第1期38-41,49,共5页
为获得联苯吡菌胺关键中间体3′,4′-二氯-5-氟-1,1′-联苯-2-胺的适合工业化生产工艺路线,对其合成工艺进行了优化。以3,4-二氯溴苯和2-溴-4-氟苯胺为原料,经格氏和Suzuki偶联2步反应合成了3′,4′-二氯-5-氟-1,1′-联苯-2-胺,其结构经... 为获得联苯吡菌胺关键中间体3′,4′-二氯-5-氟-1,1′-联苯-2-胺的适合工业化生产工艺路线,对其合成工艺进行了优化。以3,4-二氯溴苯和2-溴-4-氟苯胺为原料,经格氏和Suzuki偶联2步反应合成了3′,4′-二氯-5-氟-1,1′-联苯-2-胺,其结构经1H NMR、MS表征确证,并对合成条件进行了优化。优化条件下,3′,4′-二氯-5-氟-1,1′-联苯2-胺合成总收率61.9%,纯度98%。该工艺成本低,收率高,具有工业化生产前景。 展开更多
关键词 3′ 4′-二氯-5-氟-1 1′-联苯-2-胺 合成 联苯吡菌胺
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Synthesis,Characterization and Fluorescence Properties of Europium,Terbium Complexes with Biphenyl-4-Carboxylic Acid and o-Phenanthroline 被引量:4
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作者 赵永亮 赵凤英 +1 位作者 李强 高德青 《Journal of Rare Earths》 SCIE EI CAS CSCD 2006年第z2期18-22,共5页
Two series of solid complexes of europium and terbium with biphenyl 4-carboxylic acid and phen were synthesized and characterized in this report. Their elemental analysis, molar conductivities and TG-DTA studies indic... Two series of solid complexes of europium and terbium with biphenyl 4-carboxylic acid and phen were synthesized and characterized in this report. Their elemental analysis, molar conductivities and TG-DTA studies indicate that the complexes have the composition of Eu(phen)L3·1/2H2O, Eu0.5RE0.5(phen) L3·1/2H2O; Tb (phen) L3·H2O and Tb0.5 RE0.5(Phen)L3·1/2H2O. (RE = Y3+, La3+ and Gd3+; L = biphenyl 4-carboxylic acid; phen = o-Phenanthroline). The studies of their IR, UV 1H NMR and molar conductivities demonstrate that biphenyl 4-carboylic acid is bounded with RE (III ) ion. Rare earth ions coordinate with two nitrogen atoms of phen molecules directly in these rare earth complexes. The fluorescence spectra and fluorescence lifetimes of the rare earth complexes show that the fluorescent intensity and lifetime of a series of europium complexes are longer than those of the series of terbium complexes as having the some ligands. There are better fluorescent intensity and lifetime of hetero-nuclear rare earth complexes than homo-nuclear rare earth complexes for europium complexes. The fluorescence emission intensity of Eu3 + is raised by inert fluorescent rare earth ions (Y3+ , Gd3+ and La3+ ), but in Tb3+ hetero-nuclear rare earth complexes the intensity of Tb3+ ions are quenched by the inert fluorescent rare earth ions. 展开更多
关键词 biphenyl 4-carboxlic acid O-PHENANTHROLINE europium complex terbium complex rare earths
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Hydrothermal Synthesis,Crystal Structure and Magnetic Properties of a Novel Cobalt Complex Based on Biphenyl-3,3',4,4'-tetracarboxylate 被引量:2
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作者 陈宏 朱坤 +1 位作者 刘光祥 任小明 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 2010年第3期347-352,共6页
A novel cobalt complex,[Co2(bptc)(bix)1.5](1,H4bptc=3,3',4,4'-biphenyltetra-carboxylic acid,bix = 1,4-bis(imidazol-1-ylmethyl)benzene),has been hydrothermally prepared and characterized by IR spectroscopy,el... A novel cobalt complex,[Co2(bptc)(bix)1.5](1,H4bptc=3,3',4,4'-biphenyltetra-carboxylic acid,bix = 1,4-bis(imidazol-1-ylmethyl)benzene),has been hydrothermally prepared and characterized by IR spectroscopy,elemental analysis and single-crystal X-ray diffraction.The crystal is of triclinic system,space group P1 with a=10.770(7),b=12.245(8),c=13.514(9),α=102.829(8),β=107.734(8),γ=98.833(9)°,C37H27N6O8Co2,Mr=801.51,V=1607.5(18)3,Dc=1.656g/cm3,F(000)=818,μ=1.100mm-1,Z=2,the final R = 0.0694 and wR = 0.1543 for 3034 observed reflections(I2σ(I)).In the title complex,the two Co(Ⅱ) ions are in different coordination environments with distorted octahedral and trigonal bipyramidal geometries,respectively.The Co atoms are linked together through hexadentate bptc ligands,giving rise to 2D layers which are bridged by the bix ligands into a 3-D supramolecular network.Magnetic susceptibilities of 1 reveal weak antiferromagnetic exchange interactions between the adjacent Co(Ⅱ) ions. 展开更多
关键词 cobalt(Ⅱ) complex crystal structure biphenyl-3 3' 4 4'-tetracarboxylate
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1,5-Dimethy-4-[(3-nitro-benzylidene)-amino]-2-pheyl-1,2-dihydro-pyrazol-3-one 被引量:2
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作者 李宗孝 张新利 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 北大核心 2006年第1期29-32,共4页
The title compound C18H16N4O3 (Mr = 336.35) has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Schiff base compound is a derivative of 4-aminoantipyrine. As expect... The title compound C18H16N4O3 (Mr = 336.35) has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Schiff base compound is a derivative of 4-aminoantipyrine. As expected, the molecular structure adopts a trans configuration about the central C=N double bond. It crystallizes in orthorhombic, space group P2dc with a = 7.632(1), b = 7.816(1), c = 28.082(5) A,β = 96.18(1)°, V= 1665.48(51) A^3, Z= 4, Dc = 1.341 g/cm^3, F(000) = 704,μ = 0.094 mm^-1, the final R = 0.0448 and wR = 0.1058. Of the total 3748 collections, 3105 were unique. In the molecule there exist two different planes of pyrazoline and C(11)-C(16) phenyl ring, which are approximately coplanar (r.m.s. de deviation from the combined mean plane is 0.03 A) with the dihedral angle between them of 9.8%. 展开更多
关键词 1 5-dimethy-4-[(3-nitro-benzyllidene)-amino]-2-pheyl- 1 2-dihydro-pyrazol-3-one antipyrine derivative crystal structure
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Study the Influence of UV-Irradiation on the Photo Stability of Pure and Plasticized Poly (4-Vinyl Biphenyl) in Solid Films
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作者 Khalid Essa Al Ani Afrah Essa Ramadhan Suha Khanfar 《Materials Sciences and Applications》 2017年第13期1027-1052,共26页
The effect of UV irradiation and blending with phthalate and terephthalate plasticizers on the photo-stability of Poly (4-vinyl biphenyl) was studied at different intervals of irradiation time and in presence of air. ... The effect of UV irradiation and blending with phthalate and terephthalate plasticizers on the photo-stability of Poly (4-vinyl biphenyl) was studied at different intervals of irradiation time and in presence of air. The increase in irradiation time on the photodegradation of polymer thin films caused a change in the intensity and shape of the fluorescence band. It has been found that the stability of the polymer decreases with the increase of irradiation time, and to increases with the increase of the amount of added phthalate and terephthalate plasticizers, which is evidence of polymer photodegradation. The FT-IR spectra of irradiated pure and blended polymer with phthalate and terephthalate plasticizers showed a decrease in some absorption bands and increase in the other bands, this is also another factor for the occurrence of photo degradation of the irradiated polymer. The increase in the intensity of absorption of carbonyl and hydroxyl region, indicates a possible photogegradation of polymeric chains and the formation of alcohols, aliphatic ketones and to the increase in the number of (C=C) that resulted from hydrogen abstraction during chains-scission. 展开更多
关键词 EXCIMER Fluorescence Photodegradation Kinetics PHTHALATE Plasticizers POLY (4-Vinyl biphenyl) UV-IRRADIATION
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Synthetic Approach for Novel Fluorine Substituted <i>α</i>-Aminophosphonic Acids Containing 1,2,4-Triazin-5-One Moiety as Antioxidant Agents
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作者 Mohammed S. T. Makki Reda M. Abdel-Rahman Abdulrahman S. Alharbi 《International Journal of Organic Chemistry》 2018年第1期1-15,共15页
Novel fluorine substituted α-amino phosphonic acids containing 1,2,4-triazin- 5-one (6a-f) have been obtained from fluoroacylation of 6-(2&prime;-amino-5&prime;-nitrophenyl)-3-thioxo-1,2,4-triazin-5(4H)-one (... Novel fluorine substituted α-amino phosphonic acids containing 1,2,4-triazin- 5-one (6a-f) have been obtained from fluoroacylation of 6-(2&prime;-amino-5&prime;-nitrophenyl)-3-thioxo-1,2,4-triazin-5(4H)-one (1) followed by ammonilysis to give the corresponding 3-amino-derivative 3. Condensation of compound 3 with nitro/halogenated aromatic aldehydes yielded the Schiff bases 4. The simple addition of diethyl phosphonate to compound 4 produced the α-amino phosphonates 5. Acidic hydrolysis of compound 5 produced the fluorine substituted α-amino acids derivatives 6. Structures of the new compounds have been established with the help of elemental analysis and spectral measurements. Also, the products evaluated as antioxidants, where the fluorinated α-amino phosphonic acids 6 are more active than the other synthesized systems. 展开更多
关键词 Synthetic FLUORINE α-amino Acids 1 2 4-Triazin-5-One MOIETY ANTIOXIDANTS Activity
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Synthesis and anti-inflammatory-analgesic activity of 2',4'-difluoro-3-(carbamoyl)biphenyl-4-yl benzoates
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作者 Guang Xiang Zhong Lu Lu Chen Jian Li Wei Xiao Hu Min You Qi 《Chinese Chemical Letters》 SCIE CAS CSCD 2008年第12期1419-1422,共4页
Eighteen 2′,4′-difluoro-3-(carbamoyl)biphenyl-4-yl benzoates were synthesized from diflunisal in three steps with total yields from 72% to 86%. All compounds were identified by IR, 1^H NMR, MS and elemental analys... Eighteen 2′,4′-difluoro-3-(carbamoyl)biphenyl-4-yl benzoates were synthesized from diflunisal in three steps with total yields from 72% to 86%. All compounds were identified by IR, 1^H NMR, MS and elemental analysis. The anti-inflammatory activity and analgesic activity for 18 compounds were evaluated. The preliminary assay results showed that compounds 4a and 4p exhibited potent anti-inflammatory-analgesic activity. 展开更多
关键词 2′ 4′-Difluoro-3-(carbamoyl)biphenyl-4-yl benzoate Anti-inflammatory activity Analgesic activity DIFLUNISAL
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Synthesis and Crystal Structure of N-(Biphenyl-2-thiocarbamoyl)-4-(1,3-dichlorophenyl) Carboxamide
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作者 AAMER SAEED ULRICH FL?RKE 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 2015年第6期853-857,共5页
The synthesis of the title molecule was achieved by the reaction of 2,4-dichloro- benzoyl chloride with potassium thiocyanate in 1:1 molar ratio in dry acetonitrile to afford the corresponding isothiocyante in situ f... The synthesis of the title molecule was achieved by the reaction of 2,4-dichloro- benzoyl chloride with potassium thiocyanate in 1:1 molar ratio in dry acetonitrile to afford the corresponding isothiocyante in situ followed by the treatment with 2-aminobiphenyl. The structure of the target compound was established by elemental analysis, FTIR, 1H, 13C NMR and mass spectroscopy and unequivocally confirmed by the crystallographic data. The title compound crystallizes in the monoclinic space group P21/n with a = 13.356(2), b = 7.0761(11), c = 20.539(3) A, β = 105.723(4)°, V= 1868.5(5) A3 and Z = 4. 展开更多
关键词 synthesis crystal structure N-(biphenyl-2-thiocarbamoyl)-4-(1 3-dichlorophenyl) carboxamide
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4-[(Furan-2-ylmethylene)-amino]-1,5-dimethyl-1,2-dihyl-1,2-dihydo-pyrazol-3-one
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作者 LI Zong-Xiao ZHANG Xin-Li 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 北大核心 2005年第11期1310-1313,共4页
The title compound (C16H15N3O2, Mr= 281.31) has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Schiff base compound is a derivative of 4-aminoantipyrine. As expect... The title compound (C16H15N3O2, Mr= 281.31) has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Schiff base compound is a derivative of 4-aminoantipyrine. As expected, the molecular structure adopts a trans configuration about the C=N double bond. It crystallizes in the monoclinic system, space group P2 1/c with a = 11.150(3), b = 9.906(3), c = 13.624(4) A, β = 106.360(4)°, V= 1443.9(7) ,A^3, Z = 4, Dc = 1.294 g/cm^3, F(000) = 592,μ(MoKa) = 0.088 mm ^-1, R = 0.0577 and wR = 0.1214. Of the 5766 total reflections, 2540 were unique. In the molecule there exist two different planes of pyrazoline and O(2)-C(10) phenyl ring, which are approximately coplanar (r.m.s. de deviation from the combined mean plane is 0026 A) with the dihedral angle between them of 6.3°. 展开更多
关键词 4-[(furan-2-ylmethylene)-amino]-1 5-dimethyl-1 2-dihyl-1 2- dihydo-pyrazol-3-one crystal structure antipyrine derivative
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Synthesis and Characterization of a Novel Copoly(aryl ether ketone) Containing 4, 4'-Biphenyl-bis[4-phthalazin-1(2H)-one] Moiety
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作者 Shao Yin ZHANG Xi Gao JIAN +2 位作者 Shu De XIAO Jin Yan WANG Jie ZHANG 《Chinese Chemical Letters》 SCIE CAS CSCD 2003年第2期145-146,共2页
A new monomer of 4, 4-biphenyl-bis[4-phthalazin-1(2H)-one] was synthesized from biphenyl and phthalic anhydride, and a novel copoly(aryl ether ketone) (PPEK) was synthesized from 2, 2-bis(4-hydroxyphenyl)-propane (BPA... A new monomer of 4, 4-biphenyl-bis[4-phthalazin-1(2H)-one] was synthesized from biphenyl and phthalic anhydride, and a novel copoly(aryl ether ketone) (PPEK) was synthesized from 2, 2-bis(4-hydroxyphenyl)-propane (BPA), 4, 4'-biphenyl-bis-[4-phthalazin-1(2H)-one], 4, 4- difluorodiphenylketone (DFK). The monomer and copolymer were characterized by FT-IR and 1H-NMR. DSC and TGA were used to the novel polymer. 展开更多
关键词 Poly(aryl ether ketone) 4 4'-biphenyl-bis[4-phthalazin-1(2H)-one] 2 2-bis(4-hydroxy- phenyl)-propane(BPA).
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A Facile Synthesis of N-alkyl-4'-methyl-1,1'-biphenyl-2-sulfona-mide via Linking DoM Reaction with Suzuki Reaction
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作者 章军 周智明 +1 位作者 薛为哲 李志怀 《Journal of Beijing Institute of Technology》 EI CAS 2009年第3期327-332,共6页
Six N-alkyl-4'-methyl-1,1'-biphenyl-2-sulfonamides were synthesized facilely and efficiently from low cost and readily available benzenesulfonyl chloride and C1-C4 fatty amines via linking DoM reaction with Suzuki r... Six N-alkyl-4'-methyl-1,1'-biphenyl-2-sulfonamides were synthesized facilely and efficiently from low cost and readily available benzenesulfonyl chloride and C1-C4 fatty amines via linking DoM reaction with Suzuki reaction.The structures of the new compounds synthesized were confirmed by elemental analysis,IR,1H NMR and MS.This new method makes a feature of low cost and readily available starting material,fewer steps,mild condition,easiness to operate and higher yield. 展开更多
关键词 Do M reaction Suzuki cross-coupling reaction N-alkyl-4'-methyl- 1 l'-biphenyl-2-sulfonamide synthesis
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1-(4′-溴联苯-4-基)金刚烷的合成
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作者 赵玮 邵晓红 +9 位作者 孙建仁 潘文碧 温兴锋 陈潇 吕李章 温超群 高鋆 黄凯斌 廖飞飞 吴忠信 《精细化工中间体》 CAS 2023年第6期48-51,共4页
以1-溴金刚烷与4-溴联苯为原料,经Friedel-crafts烷基化反应制备了1-(4′-溴联苯-4-基)金刚烷。优化工艺为:反应温度25℃,反应时间24 h,1,2-二氯乙烷为溶剂,浓硫酸为催化剂,n(1-溴金刚烷)∶n(4-溴联苯)∶n(浓硫酸)=1.0∶1.0∶1.5。优化... 以1-溴金刚烷与4-溴联苯为原料,经Friedel-crafts烷基化反应制备了1-(4′-溴联苯-4-基)金刚烷。优化工艺为:反应温度25℃,反应时间24 h,1,2-二氯乙烷为溶剂,浓硫酸为催化剂,n(1-溴金刚烷)∶n(4-溴联苯)∶n(浓硫酸)=1.0∶1.0∶1.5。优化条件下目标化合物收率84.3%,纯度99.5%。目标化合物的结构经碳谱以及气相质谱表征确证。该制备方法原料易得,反应路线简单,反应条件温和,收率高,纯化处理简便,为1-(4′-溴联苯-4-基)金刚烷的工业化生产提供了新的途径。 展开更多
关键词 1-(4′-溴联苯-4-基)金刚烷 FRIEDEL-CRAFTS烷基化反应 合成
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O_3/H_2O_2处理水中4,4′-二溴联苯及其动力学研究 被引量:13
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作者 王磊 陈锦烽 +1 位作者 吕效平 韩萍芳 《环境科学》 EI CAS CSCD 北大核心 2007年第9期1998-2003,共6页
以4,4'-二溴联苯(4,4-'DBB)为代表性有机物,对比研究了单独O3和O3/H2O2处理持久性有机污染物的效能,并通过UV254值表征溶液的TOC、DOC值.结果发现,2种方法都可以达到一定的去除效果,尤其是碱性条件下H2O2的加入使去除率得到进一步提... 以4,4'-二溴联苯(4,4-'DBB)为代表性有机物,对比研究了单独O3和O3/H2O2处理持久性有机污染物的效能,并通过UV254值表征溶液的TOC、DOC值.结果发现,2种方法都可以达到一定的去除效果,尤其是碱性条件下H2O2的加入使去除率得到进一步提高.4 mg/L的4,4-'DBB溶液反应270 min后,最终去除率达到78.0%,UV254值变化率与去除率基本吻合,最终在76.9%-77.8%之间,矿化程度明显.高低2种浓度比较发现,加相同氧化剂的量,反应相同时间,去除率随溶液初始浓度增高而降低,但浓度越高的溶液的绝对处理量越大.4,4-'DBB的反应符合动力学拟一级反应规律,计算增强因子f为1.54. 展开更多
关键词 4 4'-二溴联苯 臭氧 过氧化氢 动力学
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TiO_2膜光催化降解4,4’-二溴联苯的研究 被引量:14
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作者 季彩宏 张萍 +1 位作者 韩萍芳 吕效平 《环境工程学报》 CAS CSCD 北大核心 2009年第1期72-76,共5页
研究了负载于玻璃上的固定化催化剂TiO2膜光催化降解水中4,4’-二溴联苯(4,4-’DBB)的效果,考察了溶液pH值和4,4’-DBB初始浓度等对TiO2膜光催化降解4,4’-DBB的影响,探讨了降解机理。结果表明,TiO2膜光催化降解水中4,4’-DBB的效果良好... 研究了负载于玻璃上的固定化催化剂TiO2膜光催化降解水中4,4’-二溴联苯(4,4-’DBB)的效果,考察了溶液pH值和4,4’-DBB初始浓度等对TiO2膜光催化降解4,4’-DBB的影响,探讨了降解机理。结果表明,TiO2膜光催化降解水中4,4’-DBB的效果良好,紫外光照射8 h,初始浓度为4 mg/L的4,4’-DBB的降解率高达94%,降解速率随着4,4’-DBB初始浓度的增大而下降。在溶液pH=1时,4,4’-DBB的降解效率最高。超声的加入使降解反应的速率加快。经拟合发现4,4’-DBB的降解符合拟一级反应规律,并推导出动力学方程。 展开更多
关键词 4 4’-二溴联苯 TIO2薄膜 光催化 超声
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超高效液相色谱-串联质谱法测定化妆品还原液内的4-氨基联苯 被引量:2
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作者 雷云 林雅静 +2 位作者 戴明 欧阳利群 郑小严 《分析科学学报》 CAS CSCD 北大核心 2012年第6期831-834,共4页
建立了超高效液相色谱-串联质谱(UPLC-MS/MS)检测化妆品还原液中4-氨基联苯的方法。化妆品试样经过连二亚硫酸钠化学还原后,离心、PCX固相萃取小柱提取富集、净化,并经氨化甲醇洗脱、氮吹至近干,定容后通过UPLC-MS/MS仪检测,分离柱为Wat... 建立了超高效液相色谱-串联质谱(UPLC-MS/MS)检测化妆品还原液中4-氨基联苯的方法。化妆品试样经过连二亚硫酸钠化学还原后,离心、PCX固相萃取小柱提取富集、净化,并经氨化甲醇洗脱、氮吹至近干,定容后通过UPLC-MS/MS仪检测,分离柱为Waters Acquity BEH C18柱;流动相为0.3%乙腈-甲酸水溶液;流速0.5mL/min。5种不同基质中4-氨基联苯在5~250ng/mL浓度范围内呈良好的线性关系,线性回归系数r2均大于0.999,检测限均为1ng/mL。5种不同基质中4-氨基联苯的回收率为80.9%~92.6%,相对标准偏差(RSD)为0.51%~3.76%(n=3)。 展开更多
关键词 超高效液相色谱-串联质谱法 化妆品 4-氨基联苯
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由4-联苯甲酰胺合成4-联苯腈 被引量:4
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作者 姜钦杰 王成云 +1 位作者 何庆 沈永嘉 《高校化学工程学报》 EI CAS CSCD 北大核心 2009年第1期122-125,共4页
研究了在二氯乙烷中4-联苯甲酰胺合成4-联苯腈的脱水工艺,考察了氯化亚砜用量和二甲基甲酰胺(DMF)用量等因素对该反应的影响,由此获得了较佳的反应参数:DMF的用量为4-联苯甲酰胺摩尔数的1/2,氯化亚砜为4-联苯甲酰胺摩尔数的4倍,反应时间... 研究了在二氯乙烷中4-联苯甲酰胺合成4-联苯腈的脱水工艺,考察了氯化亚砜用量和二甲基甲酰胺(DMF)用量等因素对该反应的影响,由此获得了较佳的反应参数:DMF的用量为4-联苯甲酰胺摩尔数的1/2,氯化亚砜为4-联苯甲酰胺摩尔数的4倍,反应时间5h,反应温度为80°C,如此可以75.8%的收率得到4-联苯腈。在氨气氛围中,不使用任何脱水剂,4-联苯甲酰胺可在高温(240°C)时转化成4-联苯腈,通过减压蒸馏(2~3mmHg)可以70%收率得到产物。在此反应中,温度是关键的影响因素,当温度低于220°C时,反应进展缓慢;温度高于240°C时,对提高反应速度的意义不大。 展开更多
关键词 4-联苯甲酰胺 4-联苯腈 氯化亚砜 DMF 脱水反应
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合成联苯-4-甲酸的新方法 被引量:3
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作者 王海洋 刘佳 +2 位作者 金丹 臧娜 王守凯 《化学试剂》 CAS 北大核心 2017年第3期329-332,共4页
以联苯和草酰氯为原料,通过傅克酰基化反应合成联苯-4-酮酸乙酯,经碱性水解得联苯-4-酮酸,在双氧水作用下,酮酸发生氧化脱羰基反应得目标产物。对酰化条件进行了优化并详细考察了氧化剂种类、双氧水浓度、物料配比、反应温度和时间对氧... 以联苯和草酰氯为原料,通过傅克酰基化反应合成联苯-4-酮酸乙酯,经碱性水解得联苯-4-酮酸,在双氧水作用下,酮酸发生氧化脱羰基反应得目标产物。对酰化条件进行了优化并详细考察了氧化剂种类、双氧水浓度、物料配比、反应温度和时间对氧化脱羰基反应的影响,确定较佳的工艺条件:10%双氧水作氧化剂,n(联苯-4-酮酸)∶n(双氧水)=1∶2,反应时间为3 h,反应温度为0~5℃。在此条件下,联苯-4-甲酸的收率为81.9%(以原料联苯计),纯度为99.5%(HPLC面积归一化法)。产物结构经熔点、~1HNMR和^(13)CNMR和质谱表征。 展开更多
关键词 联苯 草酰氯 联苯-4-甲酸 联苯-4-酮酸 联苯-4-酮酸乙酯
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4′-(6-溴代己氧基)-4-羟基联苯的合成 被引量:4
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作者 黄海平 何尚锦 +3 位作者 石可瑜 吴利平 杜宗杰 张保龙 《南开大学学报(自然科学版)》 CAS CSCD 北大核心 2002年第4期117-119,共3页
对合成 4′-( 6-溴代己氧基 ) -4 -羟基联苯的方法进行了改进 ,产率由 5 4 %提高到 72 % .并采取红外和核磁共振谱图表征了产物的结构 .
关键词 合成 4′-(6-溴代己氧基)-4-羟基联苯 FTIR NMR 结构表征 铁电液晶高分子材料
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4,4'-双(4-氨基苯氧基)-3,3',5,5'-四甲基联苯及其聚酰亚胺的合成与性能研究 被引量:7
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作者 虞鑫海 刘万章 +2 位作者 徐永芬 傅菊荪 赵炯心 《绝缘材料》 CAS 2008年第4期16-21,共6页
4,4'-二羟基-3,3',5,5'-四甲基联苯(TMBP)、4-氯硝基苯(4CNB)和碳酸钾在N,N-二甲基甲酰胺(DMF)和甲苯的混合溶剂体系中回流反应,合成得到了4,4'-双(4-硝基苯氧基)-3,3',5,5'-四甲基联苯(BNTMBP);随后,在Pd/C-... 4,4'-二羟基-3,3',5,5'-四甲基联苯(TMBP)、4-氯硝基苯(4CNB)和碳酸钾在N,N-二甲基甲酰胺(DMF)和甲苯的混合溶剂体系中回流反应,合成得到了4,4'-双(4-硝基苯氧基)-3,3',5,5'-四甲基联苯(BNTMBP);随后,在Pd/C-水合肼的还原体系中,被进一步还原,得到了4,4'-双(4-氨基苯氧基)-3,3',5,5'-四甲基联苯(BATMBP)。利用差示扫描量热计(DSC)、傅立叶转换红外光谱仪(FT-IR)等仪器,对其进行了表征。另外,将所得到的4,4'-双(4-氨基苯氧基)-3,3',5,5'-四甲基联苯(BATMBP)与均苯四甲酸二酐(PMDA)在强极性非质子有机溶剂中进行聚合反应,得到了粘稠状的聚酰胺酸(BATMBP/PMDA-PAA)溶液,涂膜、热亚胺化,获得了相应的聚酰亚胺(BATMBP/PMDA-PI)薄膜,并对其性能进行了研究。 展开更多
关键词 4.4’-双(4-硝基苯氧基)-3 3’ 5 5’-四甲基联苯 4 4’-双(4-氨基苯氧基)-3 3’ 5 5’-四甲基联苯 聚酰亚胺 合成 性能
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BDE-47对4种海洋微藻抗氧化酶活性的影响 被引量:22
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作者 孟范平 李卓娜 +1 位作者 赵顺顺 刘娇 《生态环境学报》 CSCD 北大核心 2009年第5期1659-1664,共6页
运用实验生态学和生物化学的方法,研究了不同质量浓度的2,2′,4,4′-四溴联苯醚(BDE-47)对海水小球藻Chlorella autotropica,牟氏角毛藻Chaetoceros muelleri,中肋骨条藻Skeletonema costatum和赤潮异弯藻Heterosigam akashiwo的抗氧化... 运用实验生态学和生物化学的方法,研究了不同质量浓度的2,2′,4,4′-四溴联苯醚(BDE-47)对海水小球藻Chlorella autotropica,牟氏角毛藻Chaetoceros muelleri,中肋骨条藻Skeletonema costatum和赤潮异弯藻Heterosigam akashiwo的抗氧化酶活性的影响。结果表明:在实验设定质量浓度范围内(0.1~2.5μg·L-1),4种微藻的超氧化物歧化酶(SOD)和过氧化氢酶(CAT)均能出现一定的应激活性,以减少BDE-47胁迫对藻细胞自身的危害,但是酶活增加的幅度却有很大不同。与赤潮异弯藻和中肋骨条藻相比,海水小球藻和牟氏角毛藻的SOD和CAT对BDE-47具有较高的敏感性。4种海洋微藻的SOD和CAT对BDE-47的敏感性顺序依次为:海水小球藻>牟氏角毛藻>中肋骨条藻>赤潮异弯藻。因此,海水小球藻的SOD和CAT可以作为指示海洋环境中BDE-47污染水平的生物标志物。 展开更多
关键词 2 2′ 4 4′-四溴联苯醚(BDE-47) 海洋微藻 超氧化物歧化酶(SOD) 过氧化氢酶(CAT)
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