Syntheses and Crystal Structures of Methyl 2-（4,5-Dibromo- 1-methylpyrrole-2-carbonylamino）-3-phenyl propanoate and 4,5-Dibromo-1-methyl-2-trichloroacetylpyrrole

1 INTRODUCTION Pyrrole and its derivatives have attracted much attention due to their chemical properties as well as biological activities[1]. They have been widely used as the materials to produce pharmaceutical, essences, biochemicals, etc. It has been found that a great deal of pyrrole derivatives present bioactivities, such as antitumor and antiviral activities[2~5]. Thus, due to the interest in exploring the syntheses of potential bioactive materials which contain pyrrole ring andna…     

Synthesis and Structure of [Cu2（μ—NO2）（aepy）4]（ClO4）3 （aepy=2—（2—Aminoethyl）pyridine）

1 INTRODUCTION There has been great and considerable interest in the study of copper nitrite complexes because they are relevant to the study of copper-containing enzymes involved in the denitrification process[1]; in particular, copper-nitrite complexes are potentially relevant to the nitrite reductases[2] (the enzyme from Achromobacter Cycloclastes) which convert NO2－ to NO and/or N2O. Many attempts have been made to synthesize a variety of copper-nitrite complexes, in which the n…     

Synthesis and Crystal Structure of Mn（phen）（PhCOO）2（H2O）

1 INTRODUCTION During the last decade the manganese che- mistry has aroused great interest due to its diverse redox functions of enzymes in photosystem Ⅱ and its specially structural, magnetic and spectroscopic properties[1, 2]. A lot of manganese complexes involving carboxylate ligands have been reported, and their properties been fully explored[3, 4]. The coordination environment of the manganese site in biosystem often consists of oxygen and nitrogen atoms from the carboxylate groups…     

Synthesis and Structure of N-（1,5-Dihydro-1-phenyl-3-methyl-4-benzoyl）-3-chloroaniline

1 INTRODUCTION 4-Acyl-5-pyrazolone, a family of flexible b- diketonate, is widely used as extract[1] and well known for its applications as analgesics, antipyre- tics, anti-inflammatory and insecticides[2]. Therefore the study on the derivation of 4-acyl-5-pyrazolone is the focus of many research groups working in the fields of coordination chemistry, biomedicine and pharmaceutical chemistry. In order to study the rela- tionship between the structure and performance of these compounds, w…     

A Convenient Synthesis of 6,8-Dimethoxy-3-[（2-（4-methoxyphenyl）ethyl）isocoumarin

6,8-Dimethoxy-3-[2-（4-methoxyphenyl）ethyl]isocoumarin was synthesized by condensation of 5,7-dimethoxyhompophthalic acid with 3-（4-methoxyphenyl）propanoyl chloride. The structure of the synthesized compound was confirmed by its mass spectrometric studies. The synthesized compound serves as a model for synthesis of DL-agrimonolide.     

Synthesis and Crystal Structure of DinuclearCadmium Complex [Cd2（phen）4（fca）2]（ClO4）2-（H2O）2

1 INTRODUCTION During the search of molecule-based materials with interesting properties such as catalysis, cla- thration etc., much attention has been focused on the synthesis of one-, two- and three-dimensional extended solids involving cadmium[1], as its d10 configuration permits a wide variety of geometries and coordination numbers. Rigid bridged ligands such as carboxylate groups are frequently used to construct these materials. Therefore, the coordi- nation chemistry of Cd(Ⅱ) ca…     

A Study on the Reaction of 1-（3-Pyridyl）-2,2-di-substituted Ethylenes with 1-Benzyl-1,4-dihydronicotinamide

The reaction of a series of 1-（3-pyridyl）-2,2-di-substituted ethylenes with 1-benzyl-1,4-dihydronicotinamide （BNAH） in deaerated acetonitrile produces the corresponding 1-（3-pyridyl）-2,2-di-substituted ethanes in contrast to benzylidenemalononitrile （BM） which does not react with BNAH under the same conditions.     

Interactions with ATP, DNA Cleavage and Anti-tumor Activities of Complexes with Anions [Mo（V）O2（O2CeH4）2]^3-, [Mo（Ⅴ）0.5W（Ⅵ）0.5O2（O2C6H4）2]^2.5- and [W（Ⅵ）O2（O2C6H4）2]^2-

(NH3CH2CH2NH2)3[Mo(Ⅴ)O2(O2C6H4)2] (1), (NH3CH2CH2NH2)2.5[Mo(Ⅴ)o.sW(Ⅵ)o.502(O2C6H4)2] (2) and(NH3CH2CH2NH2)2[VC(Ⅵ)O2(O2C6H4)2] (3) were synthesized, structurally characterized by X-ray diffraction analysis, and studied on their interactions with ATP, their DNA cleavage activities and antitumor properties. The redox state of molybdenum was not changed on going from crystal to aqueous solutions in complexes 1 and 2, while tungsten underwent reduction from W(VI) to W(V) in complexes 2 and 3. ATP promoted the oxidation of both molybdenum and tungsten from M(Ⅴ) to M(Ⅵ) and the hydrolysis of catecholate ligands in solution consisting of ATP and the complexes. Complex 1 possesses fairly good activity to DNA cleavage and against tumor S180 in mice, and is more effective than the control drug cyclophosphamide under the identical conditions. However, complexes 2 and 3 exhibited marginal effectiveness. The effectiveness of anti-tumor of the complexes was related positively to their DNA cleavage activities and their hydrolysis of catecholate ligands.     

Crystal Structure and Biological Activities of （R）-N′-[2-（4-Methoxy-6-chloro）-pyrimidinyl]- N-[3-methyl-2-（4-chlorophenyl）butyryl]-urea

1 INTRODUCTION The acyl ureas are a kind of high biological acti- vity compounds with low toxicity to mammals, birds, fish, amphibians, etc., and significant organic synthe- sis intermediates working extensively as insecticides, pesticides, fungicides and herbicides in agrochemi- cal industry[1～7]. While pyrimidinyl derivatives show excellent biological activities in the development of pesticide, and are used to develop high effective and high select herbicides. For example, pyrimidiny su…     

Synthesis and Characterization of [NH3（CH2）2NH2（CH2）2NH3]BiCl6

1 INTRODUCTION During the past decade, a series of organic-inor- ganic hybrid compounds based on metal halide units have been prepared and studied[1]. The combination of organic and inorganic components at the mole- cular level affords us the opportunity to design new hybrid materials and modulate the properties of components[2]. As a result, some interesting proper- ties, such as non-linear optical[3], interesting magne- tic[4], efficient luminescence[2], ideal thermal and mechanical sta…     

Synthesis and Crystal Structure of Tert-butyl 4-[(E)-4-(1,3 -Dioxo-1,3-dihydro-2H-isoindol-2-yl)-1-butenyl] Benzoate

1 INTRODUCTION Phthalimide and its derivatives are synthetic mate- rials, which are widely used as important chemical intermediates of biosensors[1] and many drugs such as Citalopran[2], luminal[3], Beta-Lactam[4] and the No. three generation quinolones[5], and they have been identified as active groups of some drugs and chemical luminescence reagents[6, 7]. Tert-butyl 4- [(E)-4-(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)-1- butenyl] benzoate is an intermediate of a new type of insulin sen…     

Synthesis and Crystal Structure of （Z）-Methyl-3-methoxy-2-{2-[（4-（E-3-p-tolylacryloyl）phenoxy）methyl]phenyl}acrylate

The title compound,(Z)-methyl-3-methoxy-2-{2-[(4-(E-3-p-tolylacryloyl)phenoxy)-methyl]phenyl}acrylate,was synthesized and determined by X-ray single-crystal diffraction. The crystal belongs to the triclinic system,space group P1 with a = 8.0157(8),b = 12.5748(13),c = 13.3768(14) ,α = 64.770(2),β = 75.720 (2),γ = 89.784(2)°,μ = 0.085 mm-1,Mr = 442.49,V = 1174.1(2) 3,Z = 2,Dc = 1.252 g/cm3,F(000) = 468,T = 294(2) K,R = 0.0603 and wR = 0.1498 for 2644 observed reflections with I 2σ(I). X-ray diffraction analysis reveals that the single crystal contains strong non-classical hydrogen bonds. The preliminary bioassay showed that the title compound exhibits inhibitory activity against the Pseudoperoniospora cubensis and Rhizoctonia solani at the test concentration of 200 mg/L.     

Synthesis and Crystal Structure of Trans-4-[(5-(2,4-Dichlorophenoxy)-3-methyl-1-phenyl-1H-pyrazol-4-yl)methyleneamino]-1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one

The title compound trans-4-[(5-(2,4-dichlorophenoxy)-3-methyl-1-phenyl-1H-pyra-zol-4-yl)methyleneamino]-1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 3 (C28H23Cl2N5O2, Mr = 532.41) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1 with a = 8.9438(4), b = 11.6065(5), c = 14.2215(6) , α = 112.566(1), β = 92.324(2), γ = 102.91(1)o, V = 1315.65(10) 3, Z = 2, Dc = 1.344 g/cm3, μ(MoKα) = 0.282 mm-1, λ = 0.71073 , F(000) = 552, the final R = 0.0587 and wR = 0.1578 for 5071 observed reflections (I > 2σ(I)). X-ray analysis reveals that the product is a thermodynamically stable trans isomer. Intra-and intermolecular C(12)-H(12)···O(1) and C(28)-H(28)···O(1)#1 hydrogen bonds were observed in the title compound.     

Syntheses and Crystal Structures of 4-Amino-3- （3-hyd roxyp ropyl）- 1H-1,2,4-triazole-5（4H）-thione and 6-（4-Biphenylyl）-3-（3-hydroxypropyl）-7H-1,2,4-triazolo[3,4-b][1,3,4]thiadiazine

1INTRODUCTION It has been reported that3,6-disubstituted-7H-1,2,4-triazolo[3,4-b][1,3,4]thiadiazines have a broad spec-trum of bioactivities,such as antimicrobial[1],antibac-terial,antifungal[2],anti-inflammatory[3],diuretic[4],an-thelmintic and analgesic[5].They can also be used as plant-growth regulating agents[6],photographic coup-lers,dyes for improved preservability and absorption characteristics,and inhibitors of malignant cellularZOU K.H.et al.:Syntheses and Crystal Structures o…     

Synthesis and Structure of Dinuclear Molybdenum Carbonyl Thiolate Compound[Et4N]2[Mo2(CO)8(SC6H4-CH3-p)2]

1　ＩＮＴＲＯＤＵＣＴＩＯＮＳｉｎｃｅｔｈｉｏｌａｔｅｌｉｇａｎｄｗａｓｉｎｔｒｏｄｕｃｅｄｉｎｔｏｍｏｌｙｂｄｅｎｕｍｃａｒｂｏｎｙｌｃｏｍｐｏｕｎｄｉｎ1 984 [1],ｔｈｅｉｎｖｅｓｔｉｇａｔｉｏｎｏｎｌｏｗ ｖａｌｅｎｃｅＭｏ -ＳＲｃｏｍｐｏｕｎｄｓｈａｓｒｅｃｅｉｖｅｄａｔｔｅｎｔｉｏｎｆｏｒｔｈｉｓｋｉｎｄｏｆｌｏｗ ｖａｌｅｎｃｅｃｏｍｐｏｕｎｄｓｐｏｓｓｅｓｓｃｅｒｔａｉｎａｄｖａｎｔａｇｅｏｎｃｏｍｐｏｕｎｄｓｙｎ ｔｈｅｓｉｓ,ｍｏｌｅｃｕｌｅｓｔｒｕｃｔｕｒｅａｎｄｐｈｙｓｉｃａｌａ…     

Synthesis and Crystal Structure of 2-Benzylamino-6-methyl-3-cyano-8- phenyl-5H-bispyrazolo[3,4-d,3'''',2''''-b]pyrimidine

1 INTRODUCTION The pyrazolopyrimidines have attracted conside- rable attention due to their versatile physiological activities, and a number of them exhibit excellent fungicidal[1], antiphlogistic[2～4] and antiumor[5] acti- vities. However, our interest in pyrazolo- pyrimidine stems is their applications as bactericide[6]. Herein we report the synthesis and structure of a tricyclic ring system bispyrazolo[3,4-d, 3?,2?-b]pyrimidine 1. 2 EXPERIMENTAL The 1H NMR spectra (CDCl3) were …     

Synthesis and Crystal Structure of 3-(Pyrrole-2''-carboxamido)propanoic Acid·(1/2)H2O

3-(Pyrrole-2'-carboxamido)propanoic acid I has been synthesized from the reaction of β-alanine methyl ester with 2-trichloroacetylpyrrole followed by saponifying and acidating in 85.4% yield, and the crystal structure of 3-(pyrrole-2'-carboxamido)propanoic acid· (1/2)H2O (C8H11N2O3.5, Mr = 191.19) was obtained and determined by X-ray diffraction method. The crystal is of monoclinic, space group C2/c with a = 19.010(4), b = 8.3515(17), c = 13.788(3) (A), β = 125.88(3)°, V = 1773.6(6) (A)3, Z = 8, Dc = 1.432 g/cm3, λ = 0.71073 (A), μ-MoKα) = 0.114 mm-1 and F(000) = 768. The structure was refined to R = 0.0354 and wR = 0.0942 for 1642 observed reflections with I > 2σ(I). It is revealed that the title compound has one pyrrole ring and one propionic acid subchain linked by an amido bond at C(4), and there are 8 molecules of com- pound I and 4 crystal water molecules in each unit cell. The supramolecular layers are stabilized by the hydrogen bonds of N(2) H…O(2), N(1) H…O(4), O(4) H(1W)…O(2) and O(3) H…O(1).     

Asymmetric Synthesis and Crystal Structure of （-）-N-[（3R）-3-Cyclohexyl]-3-phenylpropananoyl]bornane-10,2-sultam

The title compound (-)-N-[(3R)-3-cyclohexyl]-3-phenylpropananoyl]bornane-10,2sultam (C 25 H 35 NO 3 S,M r=429.60),a derivative of camphorsultam,crystallizes in the monoclinic space group P2 1 /c with a=10.3301(7),b=19.4040(13),c=11.8106(8),β=100.5580(10)°,V=2327.3(3) 3,Z=4,D c=1.226 g/cm 3,λ=0.71073,μ(MoKα)=0.165 mm-1 and F(000)=928.X-ray diffraction analysis reveals that the six-membered ring of sultam shows a boat form (Fig.1).The planes constructed by (C(4),C(5),C(6),C(7)) and (C(7),C(8),C(9),C(4)) form a dihedral angle of 69.5°.The C(1)-C(2)-C(3) plane forms dihedral angles to the aforementioned planes of 89.8(1) and 85.9(3)°,respectively.And molecules are linked via hydrogen bonding (C-H···N/O) interactions.     

Synthesis, Crystal Structure and Optical Properties of a New Nd(Ⅲ) Nitronyl Nitroxide Complex [Nd(NIT2Py)2(NO3)3]

A new Nd(Ⅲ) nitronyl nitroxide complex [Nd(NIT2Py)2(NO3)3] (NIT2Py = 2-(2'-pyridyl)-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide) has been synthesized and structurally characterized by X-ray diffraction.It crystallizes in monoclinic, space group P21/n with a = 12.396(4), b =11.134(4), c = 23.360(7)(。A), β = 98.178(6)°, V= 3191.2(18)(。A)3, C24H32NgNdO13, Mr = 798.83, Dc =1.663 g/cm3, μ(MoKα) = 1.704 mm-1, F(000) = 1612, Z = 4, the final R = 0.0425 and wR = 0.0957for 6532 independentreflections with Rint = 0.0642 and 4552 observed reflections (I ＞ 2σ(I)).The complex exists as discrete mononuclear molecules and the neodymium(Ⅲ) ion is ten-coordinated with three bidentate nitrate anions and two radical ligands (NIT2Py) via bidentate chelating mode.The optical properties of the complex are discussed.