Synthesis and Single Crystal X-ray Studies of 3-（3,5-Bis（trifluoromethyl）phenyl） Quinoline and 3-（4-Fluoro-3-methyiphenyl） Quinoline

The title compounds 3-（3,5-bis（trifluoromethyl）phenyl）quinoline （1） and 3-（4- fluoro-3-methylphenyl）quinoline （2） were synthesized through Suzuki-Miyaura Cross coupling reaction of 3-bromoquinoloine with aryl boronic acids. The title compounds were characterized by single-crystal X-ray diffraction, 1H NMR, 13C NMR, El-MS, elemental analysis and IR. The crystals of 3-（3,5-bis（trifluoromethyl）phenyl）quinoline （C17H9F6N, Mr = 341.25） belongs to the monoclinic system, space group P21n, a = 12.3072（13）, b = 4.9378（6）, c = 24.493（2） A, V= 1473.1（3） A3, Z = 4, Dc = 1.539 Mg m-3, 2 - 0.71073A, μ = 0.144 mm^-1, F（000） = 688, the final R = 0.0715 and wR = 0.1873 for 1875 obserwed reflections with I 〉 2σ（I） and the crystal of 3-（4-fluoro-3- methylphenyl）quinoline （C16H12FN, Mr= 237.27） belongs to the orthorhombic system, space group Pca21, a = 23.794（2）, b = 3.9094（3）, c = 25.669（2） A, V = 2387.7（4） A3, Z = 8, D, = 1.320 Mg m-3, 2 = 0.71073 A, μ = 0.088 mm-1, F（000） = 992, the final R = 0.0534 and wR = 0.1188 for 2270 observed reflections with I 〉 2σ（I）.     

Synthesis and Crystal Structure of 2-(4-Fluoro-2-(4-fluorophenoxy) phenyl)-1-(1H-1,2,4-triazol-l-ylmethyl)-3-methoxy-isopropy Alcohol

The title compound 2-(4-fluoro-2-(4-fluorophenoxy)phenyl)-1-(1H-1,2,4-triazol-z 1-ylmethyl)-3-methoxy-isopropy alcohol has been synthesized by the treatment of 1-[2-(4-fluoro-2-(4-fluorophenoxy)phenyl)-2,3-epoxypropyl]-1H-1,2,4-tdazole with sodium methoxide. It be-longs to orthorhombic, space group P212121, with a=9.7229(19), b=11.516(2), c=16.047(3) A, C18H17F2N3O3, Mr-361.35, V=1796.7(6) A3, Z=4, Dc=1.3359 g/cm3, F(000)=752,μ=0.106 mm-1, the final R=0.0329 and wR=0.0803 for 1821 unique reflections. The dihedral angles made by the triazole ring with two benzene rings are 43.56(3) and 54.78(2)°, respectively. The intermolecular hydrogen bond in the crystal lattice plays an important role in stabilizing the structure.     

Synthesis, Crystal Structure and Properties of 2,7-Bis [4-（diphenylamino）phenyl] fluorene

A novel fluorene derivative containing triphenylamine groups, 2,7-bis[4-(diphenylamino)-phenyl]fluorene (C49H36N2 , Mr= 652.80), was synthesized via Suzuki coupling reaction (yield: 19%) and its crystal structure was determined by single-crystal X-ray diffraction. It crystallizes in triclinic, space group P1 with a = 9.320(4), b = 11.250(6), c = 17.369(6) , α = 88.035(3), β = 86.450(5), γ = 73.524(5)°, V = 1742.8(13) 3 , Z = 2, Dc = 1.244 g/cm 3 , μ(MoKα) = 0.072 mm -1 , F(000) = 688, S = 1.095, the final R = 0.0616 and wR = 0.1878. It presents a linear framework constituted by a linkage of fluorene as a bridge and two triphenylamine groups. Its spectral and electrochemical properties were studied by UV-Vis absorption, fluorescence spectroscopy and cyclic voltammetry (CV). This compound can emit intense blue fluorescence with a peak wavelength of 446 nm and a full width at half maximum (FWHM) of 38 nm under UV excitation at 350 nm in film. The highest occupied molecular orbital (HOMO) energy level, the lowest unoccupied molecular orbital (LUMO) energy level and optical band gap (Eg) of the title compound are -5.46, -2.57 and 2.89 eV, respectively.     

Synthesis and Crystal Structure of 2-（4-Fluoro-2-（4-fluorophenoxy）phenyl）-1-（1H- 1,2,4-triazol-1-ylmethyl）-3-methoxy-isopropy Alcohol

The title compound 2-（4-fluoro-2-（4-fluorophenoxy）phenyl）-1-（1H-1,2,4-triazol- 1-ylmethyl）-3-methoxy-isopropy alcohol has been synthesized by the treatment of 1-[2-（4-fluoro- 2-（4-fluorophenoxy）phenyl）-2,3-epoxypropyl]-1H-1,2,4-triazole with sodium methoxide. It belongs to orthorhombic, space group P212121, with a = 9.7229（19）, b = 11.516（2）, c = 16.047（3）A, C18H17F2 N3O3, Mr = 361.35, V = 1796.7（6）A^3, Z = 4, Dc = 1.3359 g/cm^3, F（000） = 752, p = 0.106 mm^-1, the final R = 0.0329 and wR = 0.0803 for 1821 unique reflections. The dihedral angles made by the triazole ring with two benzene rings are 43.56（3） and 54.78（2）°, respectively. The intermolecular hydrogen bond in the crystal lattice plays an important role in stabilizing the structure.     

基于2，5-双(三氟甲基)对苯二甲酸配体的锌配合物的合成、晶体结构及性质

利用2,5-双（三氟甲基）对苯二甲酸（H₂L）为主配体,氯化锌为金属盐,分别与辅助配体4,4''-联吡啶（4,4''-bipy）和2,2''-联吡啶（2,2''-bipy）通过溶剂热法反应合成了配合物[Zn（L）₂（4,4''-bipy）（H₂O）]_n（1）和[Zn（L）（2,2''-bipy）]_n（2）。通过X射线单晶衍射、红外光谱、元素分析、荧光光谱、热重分析等测试手段对其结构和性质进行了表征与研究。结果表明,配合物1是以Zn²⁺为金属节点,L^2-和4,4''-bipy作为连接体相互连接,形成无限延伸的二维网状结构,层与层之间通过O5-H5B…O1氢键作用有序堆积形成三维结构。配合物2以Zn²⁺为金属节点,配体L^2-上的每个羧基都通过双齿螯合的方式桥联锌离子并无限连接形成三维网状结构。     

Synthesis and Crystal Structure of （E）-4-（3-oxo-3-（（4- （N-（pyrimidin-2-yl）-sulfamoyl）phenyl）amino）prop- 1-en-l-yl）-l,2-phenylene diacetate Dimethanol

The title compound, (E)-4-(3-oxo-3-((4-(N-(pyrimidin-2-yl)sulfamoyl)-phenyl)ami- no)prop- 1-en- 1-yl)- 1,2-phenylene diacetate dimethanol, was synthesized by the reaction of caffeic acid with sulfadiaz...     

Synthesis,Crystal Structure and Antifungal Activities of 3-Methyl-1-(4-methylphenyl)-4-(N-4-trifluoromethylphenyl)-aminomethyl-5-(4-methoxyphenylthio)-1H-pyrazole

The title compound 3-methyl-1-(4-methylphenyl)-4-(N-4-trifluoromethylphenyl) aminomethyl-5-(4-methoxyphenylthio)-1H-pyrazole has been synthesized via a four-step reaction and characterized by IR,1H NMR,elemental analysis and X-ray crystallography.The compound crystallizes in monoclinic,space group P21/c with a = 8.7170(15),b = 18.355(3),c = 15.292(3) ,β = 103.445(3)°,V = 2379.7(7) 3,Dc = 1.350 g/cm3,Z = 4,μ = 0.184,F(000) = 1008,and the final R = 0.0491 and wR = 0.1339 for 4160 observed reflections(I 2σ(I)).The results demonstrate that there is a face-to-face π-π stacking interaction between one benzene ring(C(19)~C(24)) and another(C(13)~C(18)) at a plane-plane distance of 3.3539 .The ring normal and vector between the ring centroids form an angle of 18.2o up to the centroid-to-centroid distance of 3.5273 .The crystal structure is stabilized by the intermolecular hydrogen bond of N(3)-H(3A)···N(2)(symmetry code:A –x+1,–y+1,–z).The preliminary biological test shows that the title compound has a moderate antifungal activity.     

Ring-opened Crystal Structure and Photochromism of 2,2-Bis（4-tertiary butyl phenyl）-3H-naphtho[2,1-b]pyran

The title compound, 2,2-bis（4-tertial butyl phenyl） naphthopyran, has been prepared and characterized by means of IR, ^1H NMR and elemental analysis, and its crystal structure was determined with X-ray diffraction in the ring-opened form after hydrolyzation. It belongs to monoclinic, space group P21/c, with a = 14.358（3）, b = 7.6725（15）, c = 24.470（5） А, β= 97.147（4）°, C_33H_36O2, Mr=464.62, V= 2674.8（9）А^3, Z = 4, Dc = 1.154 g/cm^3,μ= 0.070 mm^-1, F（000） = 1000, the final R = 0.0514 and wR = 0.1272 for 5444 observed reflections （I 〉 2σ（I））. X-ray analysis revealed that the C（13）-O（1） bond of the title compound cracks after UV irradiation, the six-membered heterocycles are destroyed, and zwitterionic intermediates come into being. The molecular structure in the ring-opened form is obtained after hydrolyzation. It is infrequent that the single-crystal structure is determined in a ring-opened form. A two-dimensional framework is formed by O-H…O and CAr-H…O hydrogen bonds. The UV-vis spectra show that the title compound exhibits excellent photochromic properties in solutions and polymers.     

Synthesis and Crystal Structure of 2,6-Bis（2-pyridinylmethyl）-3,5-bis（2-hydroxyl-5-chlorophenyl）pyrazine

The title compound,2,6-bis(2-pyridinylmethyl)-3,5-bis(2-hydroxyl-5-chlorophe nyl)-pyrazine(C26H12Cl2N4O2C2H8O2,Mr=551.41),has been synthesized and characterized by LC-ESIMS,NMR,UV and IR spectroscopy as well as by X-ray single-crystal diffraction.The compound behaves as a substituted pyrazine.The hydrogen atoms on C(2) and C(3) are substituted by 2-pyridinyl,whereas those on C(1) and C(4) are substituted by 2-hydroxyl-5-chlorophenyl.It crystallizes in the monoclinic system,space group P21/c with a=8.9433(12),b=32.003(4),c=10.5209(18),β=111.199(2)°,V=2807.5(7)3,Z=4,Dc=1.305 mg/m3,F(000)=1144 and μ=0.094 mm-1.A total of 13235 reflections were collected in the range of 2.17～25.01o by using a phi and omega scan mode,of which 4923 were unique(Rint=0.0692) and 2872 observed reflections with Ⅰ > 2σ(Ⅰ) were used in the structure solution and refinement.     

Synthesis and Crystal Structure of Ethyl 2,7,7-Trimethyl-4-(4＇-methylphenyl)-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate in Aqueous Medium

The title compound (C22H27NO3) was obtained by the reaction of 4-methylbenzal- dehyde, dimedone, ethyl acetoacetate and ammonium acetate in water in the presence of triethyl- benzylammonium chloride (TEBA). The crystal is of orthorhombic, space group Pbcn with a = 18.242(2), b = 15.651(1), c = 14.207(2) (A), V = 4056.15(64) (A)3, Mr = 353.45, Z = 8, Dc = 1.158 g/cm3, μ = 0.076, λ(MoKα) = 0.71073 (A) and F(000) = 1520. The final R = 0.0453 and wR = 0.0436 for 1156 observed reflections with I > 2((Ⅰ). X-ray analysis revealed that the pyridine ring is of boat conformation and the six-member ring fused with it adopts half-chair conformation.     

新型2-芳氨基嘧啶衍生物的合成

通过间羟基苯硼酸与2,4-二氯嘧啶的Suzuki反应及其后酚羟基的烷基化得到4-芳基-2-氯嘧啶衍生物. 然后, 采用Pd(PPh3)4/dppf催化剂, 在温和的条件下实现了4-芳基-2-氯嘧啶类化合物和芳香胺的偶联. 合成了3个结构新颖的2-芳氨基嘧啶类化合物. 中间体及产物的结构均经由IR, 1H NMR, 13C NMR, MS和元素分析表征而予以证实.     

Synthesis,X-ray Structure aSynthesis,X-ray Structure and Bioactivity of N-4-Methyl-1,2,3-thiadiazole-5-carbonyl-N′-3,5- dichloro-4-(1,1,2,2-tetrafluoroethoxyl)phenyl Urea

The title compound N-4-methyl-1,2,3-thiadiazole-5-carbonyl-N?-3,5-dichloro-4- (1,1,2,2- tetrafluoroethoxyl)phenyl urea (C13H8Cl2F4N4O3S, Mr = 447.19) has been synthesized from 4-methyl- 1,2,3-thiadiazole-5-carbonyl chloride as the starting material, and its structure was characterized by proton Nuclear Magnetic Resonance (1H NMR), Infra Red Spectroscopy (IR), high-resolution mass spectroscopy (HRMS), and single-crystal X-ray diffraction. The crystal of the title compound belongs to triclinic, space group P with a = 6.0780(8), b = 11.3760(14), c = 12.1440(18) , α = 96.887(7), β = 91.027(12), γ = 104.252(13)°, Z = 2, V = 806.98(19) ·3, Dc = 1.840 g/cm3, μ = 0.601 mm-1, F(000) = 448, R = 0.0450 and wR = 0.0869. X-ray analysis indicates that the 1,2,3-thiadiazole ring is not coplanar with the phenyl ring, and the dihedral angle is 33.57°. Two intermolecular hydrogen bonds N(2)-H…O(1), S(1)…H-C(11), and three weak intermolecular interactions, C(11)…O(1), N(1)…O(2) and S…O(1), are observed. The bioassay results indicate that the title compound has good insecticidal activity against Culex pipiens pallens and good induction activity for tobacco against tobacco mosaic virus which is equal to that of TDL.     

Synthesis and Crystal Structure of 1,4-Bis(2-hydroxymethylphenyl)-1,4-dioxabutane

1 INTRODUCTION Macrocyclic ligands and their metal complexes have received much attention due to their applications in ion transport, ion separation and as models in biomimic researches[1~7]. The synthetic methods of macrocyclic ligands and their metal complexes are mainly divided into three kinds[8]. The first one is synthesizing free ligand, then forming the metal complexes; the second is template synthesis; and the third is synthesizing the end-off or side-off precursor ligand, then c…     

Synthesis,Crystal Structure and Biological Activity of 2-(3,4-Dichloroisothiazol-5-yl)-4-(trifluoromethyl)-4,5-dihydrothiazol-4-yl-3-methylbenzoate

The title compound diethyl 2-(3,4-dichloroisothiazol-5-yl)-4-(trifluoromethyl)-4,5-dihydrothiazol-4-yl-3-methylbenzoate(C15H9Cl2F3N2O2S2, Mr = 441.26) was prepared from methyl 3,4-dichloroisothiazole-5-carboxylate as the starting material by four steps of reaction. Its structure was characterized by IR, 1H-NMR, 13C-NMR, EA and single-crystal X-ray diffraction. The crystal of the title compound belongs to the monoclinic system, space group P21/c with a = 8.8437(18), b = 16.128(3), c = 12.305(3), β = 91.68(3)o, V = 1754.4(6) 3, Z = 4, Dc = 1.671 g/cm3, μ(Mo Ka) = 0.71073 mm-1, F(000) = 888, R = 0.0384 and w R = 0.0778. Weak π-π interactions occur between the isothiazole rings and phenyl rings of adjacent molecules to form a one-dimensional chain and stabilize the crystal structure. Bioassay indicates that the title compound has good activity against the fungi and TMV tested.     

2,2,7,7-四甲基-5,6-二氧代-9-(2-氯苯基)-10-(4-甲基苯基)-9,10-二氢-2H-吖啶的合成和晶体结构

标题化合物2,2,7,7-四甲基-5,6-二氧代-9-(2-氯苯基)-10-(4-甲基苯基)-9,10-二氢-2H-吖啶(C30H32ClNO2,Mr=474.02)是由邻氯苯甲醛和5,5-二甲基-1,3-环己二酮和对甲基苯胺以乙二醇作溶剂在微波辐射下而得到的。结构通过单晶X-射线衍射分析确定,其晶体属于单斜晶系,空间群P21/c,a=12.048(3),b=11.044(2),c=19.989(5)?b=101.42(2),Z=4,V=2607(1)3,Dc=1.208g/cm3,m(MoKa)=0.173mm-1,F(000)=1008,R=0.0450,wR=0.0869。X-射线衍射分析表明:原子C(8),C(13),C(14),C(15),C(20)和N形成1个六员环,采用船式构象,六员环C(8)~C(13)和C(15)~C(20)采用半椅式构象。     

新的含有4-对甲基苯基-3，5-二(2-吡啶基)-1，2，4-三氮唑钴配合物的合成和晶体结构(英)

A new cobalt(Ⅱ) complex, [CoL₂(NCS)₂]·2CH₂Cl₂, [L=4-(p-methylphenyl)-3,5-bis(pyridin-2-yl)-1,2,4-triazole], was synthesized and its crystal structure was determined by X-ray analysis. The complex crystallizes in monoclinic system with space group P2₁/c, a=0.867 40(17), b=1.453 9(3), c=1.781 9(4) nm, β=91.18(3)°, V=2.246 7(8) nm³ and Z=2. The cobalt atom is in a distorted octahedral environment with two bidentate chelating L ligands in the equatorial plane and two NCS^- ions in the axial positions. CCDC: 251658.     

3-[3-甲氧基-4-(2-乙氧基-2-氧代乙氧基)苯基]丙烯酸乙酯的合成及其晶体结构

以香草醛为原料,经Williamsom反应和Knoevenagel-Doebner反应制得新化合物3-(3-甲氧基-4-羧甲氧基苯基)丙烯酸(2);2与乙醇经酯化反应合成了阿魏酸衍生物——3-[3-甲氧基-4-(2-乙氧基-2-氧代乙氧基)苯基]丙烯酸乙酯(3),其结构经1H NMR,IR,元素分析和X-射线单晶衍射确证。3属三斜晶系,空间群P-1,晶胞参数a=8.301,b=8.474,c=11.445,α=82.94°,β=86.86°,γ=84.52°,V=794.63,Z=2,Dc=1.289 g·cm-3,R1=0.046 7,wR2=0.101 8。3通过分子间氢键(C-H┈O)形成了二维网状结构。     

Synthesis and Crystal Structure of（E）-Ethyl 2-（5-（3-methyl-2-butenyloxy）-2-（3-（4-（3-methyl-2-butenyloxy）phenyl）acryloyl）phenoxy）acetate

The title compound,(E)-ethyl 2-(5-(3-methyl-2-butenyloxy)-2-(3-(4-(3-methyl-2-butenyloxy)phenyl) acryloyl) phenoxy)acetate(1),has been synthesized and characterized by FT-IR and 1H-NMR spectroscopy,ESI-MS,and X-ray single-crystal diffraction.FT-IR,1H-NMR and ESI-MS confirm the functional groups,particularly the ethyl groups in the ester moiety,of the compound.The single-crystal X-ray diffraction has revealed a monoclinic structure,space group P21/n with a = 14.6832(14),b = 7.7581(7),c = 23.075(2),β = 101.670(2)o,V = 2574.2(4) ?3,Z = 4,Dc = 1.235 g/cm,μ = 0.085 mm-1,and F(000) = 1024.The skeleton of chalcone in the molecular structure is coplanar.     

Synthesis and Crystal Structure of (Z)-Ethyl-4-(4-methoxy)benzylidene-2-(3,5-dimethoxypheny-tetrahydrofuran-3,3-dicarboxylate

The title compound (Z)-ethyl-4-(4-methoxy)benzylidene-2-(3,5-dimethoxyphenyl)- tetrahydrofuran-3,3-dicarboxylate has been synthesized, and its crystal structure was characterized by X-ray single-crystal diffraction. The crystal belongs to triclinic, space group P1-, with a = 8.140(3), b = 11.966(4), c = 13.771(5) α = 67.366(4), β = 85.165(5), γ = 75.806(4)°, V = 1200.1(7) 3, Z = 2, C26H30O8, Mr = 470.50, Dc = 1.302 g/cm3, F(000) = 500, λ(MoKα) = 0.71073 , μ = 0.096 mm–1, R = 0.0659 and wR = 0.1841 for 3080 observed reflections (I > 2σ(I)). As a key intermediate of HIV-1 integrase inhibitor, the synthesis and structure confirmation of the title compound are important for further studies.