A New Luminescent Cd(Ⅱ) Coordination Polymer Constructed with 2-(Carboxymethoxy) benzoic Acid

In this work, we synthesized a new Cd（Ⅱ） coordination polymer, [Cd（L）(cmb)H;O]· H;O（1）, by using mixed 2-（carboxymethoxy）benzoic acid（H2 cmb） and typical chelating N-donor ligands 2-（2-fluoro-6-fluorophenyl）-1 H-imidazo[4,5-f][1,10]phenanthroline ligand（L）. 1 crystallizes in monoclinic, space group P21/c with a = 17.6150（8）, b = 9.7811（4）, c = 18.1603（8） ?, β = 118.9150（10）o, V = 2738.9（2） ?;, Z = 4, C28 H20 CdF2 N4 O7, Mr = 674.88, Dc = 1.637 g/cm3, F（000） = 1352, μ（Mo Ka） = 0.865 mm–1, R = 0.0643 and w R = 0.1976. In 1, the cmb2– anions link neighboring Cd（Ⅱ） atoms in a bis-chelating mode, yielding a one-dimensional chain structure along the b axis. The L ligands are attached on one side of the chain through chelating the Cd（Ⅱ） atoms, and are stacked with those of an adjacent chain through π-π interactions to generate a one-dimensional double-chain structure. Furthermore, the one-dimensional double-chains are stacked by C–H???π interactions between the carbon atom of L ligand and the benzene ring of cmb2–ligand to give a layer structure. Moreover, the solid state luminescent property of 1 was also investigated at room temperature.

Effect of manganese and potassium addition on CeO_2-Al_2O_3 catalyst for hydrogenation of benzoic acid to benzaldehyde

A series of Mn/CeO2-Al2O3 and K/CeO2-Al2O3 catalysts for hydrogenation of benzoic acid to benzaldehyde were prepared to in- vestigate the effect of Mn, K addition on CeO2-Al2O3 catalyst. X-ray diffraction (XRD) and H2-temperature-programmed reduction (H2-TPR) results suggested that the interaction between CeO2 and MnOx enhanced the reducibility of catalysts and therefore benzoic acid conversion. The addition of K increased the number of basic number on the catalyst which leads to a high selectivity to benzaldehyde, but excessive addition imposed negative effects on the catalyst performance. A Mn-K/CeO2-Al2O3 catalyst was developed and investigated in the reaction. The simultaneous addition of Mn and K enhanced not only the catalytic activity but also the capacity to resist the coke formation over catalyst.

A Green Synthesis of 2-Ethylanthraquinone by Dehydration of 2-(4'-ethylbenzoyl) benzoic Acid over Solid Acid Catalysts

The dehydration of 2-（4＇-ethylbenzoyl） benzoic acid （BE acid） to 2-ethylanthraquinone （2-EAQ） was investigated over solid acid catalysts. The results showed that H-beta zeolite catalyst modified by dilute HNO3 solution exhibited an excellent performance. In our study, the conversion of BE acid can reach 96.7%, and the selectivity to 2-EAQ is up to 99.6%.

Two Tetranuclear Zinc(Ⅱ) Coordination Polymers Based on 3,5-Bis(2-carboxylphenoxy)benzoic Acid with Highly Selective Sensing of Nitrobenzene

Two novel zinc（Ⅱ） coordination polymers, [Zn2（BCB）（CH3OH）（μ3-OH）]n（1） and {[Zn2（BCB）（μ3-OH）（H2O）2]·CH3OH}n （2）, have been constructed from 3,5-bis（2-carboxylphenoxy）benzoic acid（H3BCB） and characterized by elemental analysis（EA）, IR, powder X-ray diffraction（PXRD）, and thermogravimetric（TG） analyses. Structural analysis reveals that complexes 1 and 2 are both 1D polymeric chains with unprecedented tetranuclear {Zn4（COO）4（μ3-OH）2} clusters, which were further expanded into a 2D structure. Fluorescence measurements show that 1 and 2 have highly selective and sensitive detection of nitrobenzene.

Structures and Properties of Two Pb^Ⅱ Compounds and Theoretical Study of 2,4-Oxybis（benzoic acid）

Two Pb^Ⅱ coordination polymers [Pb（oba）（2,2′-bipy）]·1.5H2O（1） and [Pb（oba）（phen）]（2）（H2oba = 2,4-oxybis（benzoic acid）, 2,2′-bipy = 2,2′-bipyridine, phen = 1,10-phenanthroline） were synthesized by hydrothermal reactions and characterized by single-crystal X-ray diffraction, thermogravimetric analyses, IR spectroscopy and elemental analysis. Structures of compounds 1 and 2 are similar. Compounds 1 and 2 show 1D wavy chains, which are further connected through aromatic π-π stacking interactions to expand into 2D wavelike networks. The crystal structure of 2,4-oxybis（benzoic acid） ligand（3） was obtained, and its full geometry optimization was carried out by using DFT methods at the B3LYP/6-31G（d） level. The calculated data show that the bond distances and bond angles were very close to the experimental data. The values of the frontier orbital energies indicate that this configuration is stable. Moreover, the solid-state fluorescence properties of 1-3 have also been investigated.

Synthesis, Crystal Structure, Luminescent Property and DNA-Binding of a Cadmium Complex with 2,4-Bis-oxyacetate-benzoic Acid

A complex [Cd2Na2（BOABA）2（H2O）8]·H2O（1） was synthesized by using 2,4-bisoxyacetate-benzoic acid（H3BOABA） and Cd（OH）2. It was characterized by elemental analysis, IR spectra, and single-crystal X-ray diffraction. Complex 1 shows a two-dimensional 3-connected rigid plane. The interactions between the ligand and its complex with DNA were studied by Et Br fluorescence probe. Photoluminescent studies indicate that the complex may be excellent candidates for potential photoactive materials.

One-pot synthesis of 2-(1-acyloxypentyl)benzoic acids

A one-pot synthesis of 2-（1-acyloxypcntyl） benzoic acids by trapping the carboxylatc/alkoxide dianion with acylating reagents following Grignard addition with n-BuMgBr to 2-formylbcnzoic acid was described. Compared with routine synthetic method, this novel procedure has the advantage of convenient operation and higher yields.

Metal-organic frameworks derived from divalent metals and 4-(1H-1, 2, 4-triazol-1-yl)benzoic acid

Two inorganic-organic coordination polymers, [Cd(TBA)2]·3H2O (1) and [Cu(TBA)2]·2H2O (2) have been synthesized by reaction of the metal ions of Cd(II) and Cu(II) with the ligand HTBA [HTBA = 4- (1H-1, 2, 4-triazol-1-yl)benzoic acid] under solvothermal condition. The compounds were characterized by single-crystal X-ray diffraction, elemental analysis, IR spectroscopy, X-ray powder diffraction (XRPD), and thermo gravimetric analysis (TGA). The structural analyses reveal the two independent polymers exhibit different structures. Complex 1 exhibits a 3D framework with 1D channels, and complex 2 shows a 2-fold interpenetrating 3D diamond net.

Synthesis and Crystal Structure of 2-[(4-Methoxy- 6-methylthio-2-pyrimidinyl)aminocarbonyl- aminosulfonyl] Benzoic Acid Methyl Ester

The title compound 2-[(4-methoxy-6-methylthio-2-pyrimidinyl)aminocarbonyl- aminosulfonyl]benzoic acid methyl ester (C15H16N4O6S2, Mr = 412.44) was obtained by the reaction of (4-methoxy-6-methylthio-2-pyrimidinyl)amine with 2-methoxylcarbonylbenzene-sulfonylisocya- nate. The crystal is of monoclinic, space group P21/c with a =11.169(3), b = 9.508(3), c = 17.690(5) ? b = 91.593(5), Z = 4, V = 1877.9(10) 3, Dc = 1.459 g/cm3, F(000) = 856, m(MoKa) = 0.324 mm-1, R = 0.0690 and wR = 0.1368 for 3301 observed reflections (I > 2s(I)). The N(1)H…N(3) and N(2)H…O(4) hydrogen bonds can be observed. In the molecule the phenyl plane(I), pyrimi- din-2-yl-urea bridge plane(Ⅱ) and ester plane(Ⅲ) form three conjugated systems.

Effects of benzoic acid(Vevo Vitall) on the performance and jejunal digestive physiology in young pigs

Background： As a organic acid, benzoic acid has become one of the most important alternatives for antibiotics,and its beneficial effect on performance in animals has been proven for a decade. However, knowledge of the effects of benzoic acid on jejunal digestive physiology, especially the antioxidant capacity and mucosal glucagon-like peptide2（GLP-2） concentrations is lacking.Methods： A total of 20 barrows [Duroc ×（Yorkshire × Landrace）] with an average body weight（BW） of 18.75 ± 0.2 kg were used in a 14-d trial to determine the potential mechanisms of benzoic acid supplementation on the performance,nutrient digestibility and jejunal digestive physiology in young pigs. All pigs were randomly allotted to 1 of 2 diets supplemented with 0 or 5000 mg/kg benzoic acid.Results： Relative to the control, benzoic acid supplementation increased the average daily feed intake（ADFI）, and average daily gain（ADG） in young pigs（P 〈 0.05）, improved the apparent total tract digestibility of dry matter（DM）,crude protein（CP）, ether extract（EE）, gross energy（GE） and crude ash（P 〈 0.05）, and enhanced the activities of trypsin,lipase and amylase in the jejunum（P 〈 0.05）. Similarly, relative to the control, supplementing benzoic acid in the diet resulted in a trend to reduce the p H values of the digesta（P = 0.06）, decreased crypt depth and increased the villus height to crypt depth ratio（P 〈 0.05） in the jejunum of pigs. Finally, benzoic acid supplementation increased the mR NA expression and concentration of glucagon-like peptide 2 and the activities of glutathione peroxidase and superoxide dismutase in the jejunal mucosa of young pigs（P 〈 0.05）.Conclusions： In conclusion, supplementation with 5000 mg/kg benzoic acid improved the performance of young pigs through promoting nutrient digestion, improving jejunal antioxidant capacity, and maintaining the jejunal morphology in young pigs.

Synthesis, Structure and Photoluminescence of a New Cd(Ⅱ) Coordination Polymer Based on 4-(Carboxymethoxy)-benzoic Acid and 1,10-Phenanthroline Derivative

A new ID coordination polymer, [Cda（L1）2（L2）2].H2O （1, H2L1 = 4-（carboxy- methoxy）benzoic acid and L2 = 2-（4-fluorophenyl）-I H-imidazo[4,5-f][1,10]phenanthroline）, has been hydrothermally synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. It crystallizes in triclinic, space group P1 with a = 9.985（5）, b = 10.768（5）, c = 12.512（5） A, a = 68.959（5）, β = 80.354（5）, γ = 79.663（5）°, V= 1227.4（10） A3, Z = 1, C56H36Cd2F2N8O11, Mr = 1259.73, Dc = 1.704 g/cm3, F（000） = 630, μ（MoKa） = 0.949 mm-1, R = 0.0261 and wR = 0.0655. The L1 anions link the neighboring Cd（II） atoms to form a 1D double chain structure. The L2 ligands are alternately located on both sides of the double chains. More interestingly, the lateral L2 ligands from adjacent double chains are paired to furnish strong π-π interactions, yielding a 2D supramolecular layer. N-H...O, O-H...N and O-H...O hydrogen bonds further stabilize the structure of 1. The luminescent property of 1 was studied in solid state at room temperature.

2-(乙酰氧基)苯甲酸的HPLC分析方法建立及优化中的几点思考

本文在建立2-(乙酰氧基)苯甲酸的HPLC分析方法过程中,对溶剂对样品的稳定性影响,梯度或等度洗脱的差异,以及特异性参数设置对纯度因子的影响进行了研究。结果表明,在溶剂和流动相中适量加入冰乙酸能有效抑制2-(乙酰氧基)苯甲酸分解为水杨酸;梯度洗脱尽管能产生比等度洗脱峰形更好、峰宽更窄的色谱峰,但梯度洗脱时,流动相中的乙酸会影响方法特异性。方法最终以甲醇和0.1%冰乙酸溶液为流动相,在276 nm的检测波长下,对99%2-(乙酰氧基)苯甲酸原药及30%2-(乙酰氧基)苯甲酸可溶粉剂进行分析。方法确证结果表明该方法满足制剂中2-(乙酰氧基)苯甲酸检测要求。

有机酸改性Hβ沸石催化剂上2-(4′-乙基苯甲酰基)苯甲酸脱水闭环合成2-乙基蒽醌

采用柠檬酸等有机酸对Hβ沸石样品进行改性,研究了改性后Hβ沸石样品在2-(4′-乙基苯甲酰基)苯甲酸(BEA)脱水闭环合成2-乙基蒽醌(2-EAQ)反应中的催化性能.采用X射线衍射、X射线荧光光谱、红外光谱、核磁共振和程序升温脱附方法对催化剂进行了表征.结果表明,有机酸改性没有破坏Hβ沸石样品的骨架结构,但其有序度和结晶度均有不同程度的降低,而且酸量明显减少;其中草酸改性后的催化剂脱铝严重.柠檬酸、酒石酸、苹果酸和丙二酸改性后的Hβ沸石样品在合成2-EAQ的反应中有较好的反应性能,以其为催化剂,BEA的转化率和2-EAQ的选择性均在95.0%以上.

柠檬酸改性的H-Beta上2-(4′-乙基苯甲酰基)苯甲酸的脱水反应(英文)

以改性的H-beta沸石分子筛为催化剂,代替传统的浓硫酸或发烟硫酸催化剂,使2-(4′-乙基苯甲酰基)苯甲酸脱水闭环生成2-乙基蒽醌是一条清洁生产路线.其中柠檬酸改性的H-beta催化剂表现出很好的催化性能,可以明显降低反应温度,缩短反应时间.在柠檬酸改性的H-beta催化剂上,当反应温度为529 K,反应时间为60 min时,2-(4′-乙基苯甲酰基)苯甲酸的转化率为99.5%,2-乙基蒽醌的选择性可达97.2%;而在未经柠檬酸改性的H-beta催化剂上,当反应温度为550 K,反应时间为60 min时,2-(4′-乙基苯甲酰基)苯甲酸的转化率只有81.6%,2-乙基蒽醌的选择性为96.4%.

柠檬酸浸渍改性H-β沸石对2-(4＇-乙基苯甲酰基)苯甲酸脱水合成2-乙基蒽醌反应的催化性能

采用浸渍法制备了柠檬酸改性的H-β沸石催化剂,采用X射线衍射、X射线荧光、红外光谱、核磁共振和程序升温脱附方法对催化剂进行了表征,并考察了催化剂对2-(4′-乙基苯甲酰基)苯甲酸(EBA)脱水合成2-乙基蒽醌(EAQ)反应的催化性能.结果表明,经柠檬酸改性没有破坏H-β沸石的骨架结构,但其酸量明显减少.柠檬酸浸渍改性后未经水洗的催化剂上有较多的非骨架铝及柠檬酸残留;水洗至中性的催化剂在EBA脱水合成EAQ反应中有较好的催化性能,EBA转化率可高达96.5%,EAQ选择性可高达96.0%.

Yb(NTf_2)_3催化苯甲酸酯化反应

报道了三 (双 (三氟甲基磺酰亚胺 ) )镱———Yb(N(SO2 CF3) 2 ) 3(简称Yb(Ntf2 ) 3)催化苯甲酸与乙醇、异丙醇、叔丁醇和二甘醇的直接酯化反应。研究了反应时间、温度、酸醇摩尔比、催化剂用量等对苯甲酸酯化反应的影响。得到Yb(NTf2 ) 3催化合成苯甲酸乙酯的最佳条件是催化剂采用摩尔分数为 8% ,n(酸 )∶n(醇 ) =1∶7,回流 6h ,不分水 ,产率为 99%。考察了醇结构对酯化反应的影响 。

2-(4-氟代苯甲酰基)苯甲酸-铕配合物的合成、结构表征及荧光性能的研究

以硝酸铕、2-（4-氟代苯甲酰基）苯甲酸（HL）、1,10-菲咯啉（Phen）和三苯基氧膦（TPPO）合成了EuL3（H2O）6,EuL3Phen（H2O）4和EuL3（TPPO）（H2O）5三种固态配合物。用元素分析、红外光谱、核磁共振氢谱对配合物进行了组分确定和结构表征。IR表明,2-（4-氟代苯甲酰基）苯甲酸与Eu^3＋形成配合物后,位于1 692 cm^-1处羧基的νC O峰消失,2 500-3 200 cm^-1处羧基的νO—H峰也消失,出现了羧酸盐特有的反对称伸缩振动吸收峰（aνs（CO2^-））和对称伸缩振动吸收峰（sν（CO2-））,且Δν（aνs（CO2^-）-sν（CO2^-））与钠盐的Δν相近,说明羧酸根与Eu^3＋以对称双齿桥式配位。在1H NMR中,形成配合物后第一配体苯环上的质子峰变为宽峰且移向高场,Phen和TPPO中质子化学位移移向低场。室温下测定了配合物的荧光激发光谱和发射光谱,激发光谱表明配合物EuL3（H2O）6,EuL3Phen（H2O）4和EuL3（TPPO）（H2O）5的最佳激发波长分别为353.0,355.0和357.0 nm;发射光谱均显示Eu^3＋离子的特征发射光谱,且表明Phen对Eu3＋离子的荧光发射有明显增强作用。

Hβ沸石催化剂酸性及晶粒尺寸对2-(4′-乙基苯甲酰基)苯甲酸脱水闭环反应的影响

采用4种不同硅/铝比(n(SiO2)/n(Al2O3))β沸石经柠檬酸改性制备了4种催化剂。采用XRF、XRD、NH3-TPD和SEM等方法对催化剂进行了表征。并将它们用于2-(4′-乙基苯甲酰基)苯甲酸(BEA)脱水闭环合成2-乙基蒽醌(2-EAQ)反应,考察其催化性能。结果表明,在较低反应温度(230℃)下,4种催化剂样品的活性差别很大,n(SiO2)/n(Al2O3)=25的催化剂样品上反应物BEA的转化率为82.2%,而n(SiO2)/n(Al2O3)=38的催化剂样品上BEA的转化率仅为30.3%;在较高反应温度(258℃)下,4种催化剂样品的活性差别较小。结果还表明,β沸石的酸性质对催化剂的催化性能有一定影响,而催化剂晶粒尺寸对其催化性能影响较大,晶粒小,扩散容易,反应活性高;反之,活性较低。

2-(4′-乙基苯甲酰基)苯甲酸催化脱水闭环反应中Hβ沸石催化剂失活和再生的研究

研究了柠檬酸改性的Hβ沸石催化剂在2-(4′-乙基苯甲酰基)苯甲酸(BEA)脱水闭环合成2-乙基蒽醌(2-EAQ)工艺中的失活及再生性能。结果表明,催化剂经过多次重复使用,催化活性下降。通过乙醇洗涤催化剂再焙烧的方法,可以恢复催化剂活性。再生后的催化剂重复使用4次后,BEA的转化率仍然高达99.5%,2-EAQ选择性也高达99.4%。采用TG-DTA对乙醇洗涤前后失活催化剂进行表征,并结合电喷雾质谱API-ES和1HNMR对催化剂上积炭物种的组成进行了定性分析。

新显色剂2-(2'-咪唑偶氮)-苯甲酸与铜(Ⅱ)的显色反应研究

研究了新显色剂 2 ( 2′ 咪唑偶氮 ) 苯甲酸 (简称 IABA)与铜 ( )的显色反应条件。结果表明 ,在 p H 7的醋酸铵介质中 ,试剂与铜 ( )形成稳定的紫红色的配合物 ,最大吸收波长为 5 44nm,铜 ( )与试剂 IABA的配合比为 1∶ 2 ,表观摩尔吸光系数为 1.5 3× 10 4L mol· cm,铜 ( )浓度在 0～ 0 .8mg L范围内遵守比耳定律。该方法用于测定镁合金和铝合金中微量的铜 ,结果满意。