Synthesis,spectroscopic characterization,biological screening,and theoretical studies of organotin(IV) complexes of semicarbazone and thiosemicarbazones derived from (2-hydroxyphenyl)(pyrrolidin-1-yl)methanone

Research on Chemical Intermediates - New organotin(IV) complexes of (2-hydroxyphenyl)(pyrrolidin-1-yl)methanone thiosemicarbazone [L1H2], (2-hydroxyphenyl)(pyrrolidin-1-yl)methanone...     

Synthesis and Characterization of Reactive Poly(Aryl Ether Ketone Ketone) Containing Cyclohexene Ring

Poly(aryletherketone)sareoneofthemostimportanthighperformanceengineeringthermoplastics,widelyusedinelectronic,electric,aircraft,andaerospaceindustries.Initially,considerableeffortwasmadetomodifytheirchemicalstructure,essentiallytoimprovetheirthermalproperties'.Inthelastfewyears,moreattentionwaspaidtotheirfunctionalization2.Thiscanbeachievedeitherbychemicalmodificationofthepolymerorbydirectsynthesisusingfunctionalizedmonomers.Inthisletter,wesynthesizedanovelmonomer4byintroducingcyclohexeneringa…     

（4-羟基-2-甲基苯基）（2-羟基苯基）甲酮的合成、晶体结构与紫外吸收

用水杨酸和间甲酚为原料,在三氯氧磷和氯化锌的作用下合成了（4-羟基-2-甲基苯基）（2-羟基苯基）甲酮（C14H12O3）,通过IR、NMR、元素分析、X射线单晶衍射等手段对化合物进行了结构表征．该晶体属于单斜晶系,空间群为P2（1）／n,晶胞参数为：a=1．09534（10）,b=0．84616（6）,c=1．30458（19）nm,α=γ=90°, β=109.584 （2）°, V=1. 139 2（2） nm^3, Z=4, Mr =228.24, Dc =1.331 g/cm^3, μ=0.093 mm^-1, F （000） =480,羟基和羰基中的氧原子所形成的分子问氢键把分子连接成一维链．该化合物在240～360nm之间有强烈的紫外吸收．     

Synthesis and Crystal Structure of (3,6-Dichloro-2-nitrophenyl)(3-nitrophenyl)methanone

Novel compounds, (3,6-dichloro-2-nitrophenyl)(3-nitrophenyl)methanone(2), (2-amino-3,6-dichloro- phenyl)(3-aminophenyl)methanone(3) and 1-[3-(2-amino-3,6-dichlorobenzoyl)phenyl]-1H-pyrrole-2,5-dione(4), were synthesized from the initial compound 2,5-dichlorobenzophenone(1) and characterized by 1H NMR, 13C NMR, IR, mass spectrum and element analysis, respectively. The single crystal of compound 2 was obtained and determined by X-ray diffraction analysis. The single crystal data illustrates that it belongs to...     

Zeolite-catalyzed synthesis of nicotinyl-fused indolo-pyrazoles and evaluation of their activities against Anopheles arabiensis and Lipoxygenase

A series of nicotyl-fused indolo-pyrazoles (NFIPs) were synthesized by a one-pot multicomponent reaction of aryl aldehydes, isoniazid, and indole in the presence of zeolite as a catalyst. Structures of all the synthesized compounds were established by IR, ¹H-NMR, ¹³C-NMR, 2D-NMR, TOF-MS, and elemental analysis. The products were obtained in excellent yields and high purity. All 10 compounds were screened for larvicidal and insecticidal properties against Anopheles arabiensis and tested for their lipoxygenase inhibitory activity. Compounds (3-(3-hydroxy-4-methoxyphenyl)-2,3-dihydropyrazolo[4,3-b]indol-1(4H)-yl)(pyridin-4-yl)methanone ( 4i ) and (3-(3-bromo-5-hydroxy-4-methoxyphenyl)-2,3-dihydropyrazolo[4,3-b]indol-1(4H)-yl)(pyridin-4-yl)methanone ( 4j) displayed highest larvae mortality at a 4 μg/ml dose in 24 h. Compounds (3-(4-methoxyphenyl)-2,3-dihydropyrazolo[4,3-b]indol-1(4H)-yl)(pyridin-4-yl)methanone ( 4h ) and (3-(3-hydroxy-4-methoxyphenyl)-2,3-dihydropyrazolo[4,3-b]indol-1(4H)-yl)(pyridin-4-yl)methanone ( 4i ) showed a significant knockdown activity after 24 h with 70% mortality. Furthermore, (3-(4-chlorophenyl)-2,3-dihydropyrazolo[4,3-b]indol-1(4H)-yl)(pyridin-4-yl)methanone ( 4c ) and (3-(3-bromo-5-hydroxy-4-methoxyphenyl)-2,3-dihydropyrazolo[4,3-b]indol-1(4H)-yl)(pyridin-4-yl)methanone ( 4j ) displayed promising lipoxygenase inhibitory activity with a mortality of 70% and 60%, respectively.     

含二羟基二苯酮热致液晶共聚酯的合成与表征（Ⅵ）──含二羟基二苯酮热致液晶共聚酯结晶结构的X射线衍射研究

以广角Ｘ－射线衍射（ＷＡＸＤ）对含二羟基二苯酮（ＢＨＰ）、对羟基苯甲酸（ＰＨＢＡ）、对苯二甲酸（ＴＰＡ）、问苯二酚（ＲＥＳ）的系列热致液品共聚酯进行了较为深入的研究，详细讨论了不同组成的共聚酯的结晶结构、结晶度、结晶颗粒大小等等。     

含4，4＇－二羟基二苯酮热致液晶四元共聚酯的合成与表征

含４，４＇－二羟基二苯酮热致液晶四元共聚酯的合成与表征董德文，韩平，倪玉山，丁孟贤，韩伟（中国科学院长春应用化学研究所长春１３００２２）（吉林化工学院化工系吉林）关键词　热致液晶，共聚酯，向列型，二羟基二苯酮关于热致液晶芳香族聚酯的研究已有大量的报道...     

Synthesis and Crystal Structure of （5-Hydroxy-6-methoxybenzofuran- 3-yl）-（4-methoxyphenyl）methanone

Compound 1 (5-hydroxy-6-methoxybenzofuran-3-yl)(4-methoxyphenyl)methanone, C17H14O5 , as a potential anti-breast cancer agent has been synthesized under microwave irradiation, which was further converted to (5,6-dihydroxybenzofuran-3-yl)(4-methoxyphenyl)methanone (2). The compounds were characterized by MS and NMR spectra. Meanwhile, the crystal of 1 was obtained and determined by X-ray single-crystal diffraction. Crystal data: monoclinic system, space group P21/n, a=8.908(6), b=10.505(7), c=15.452(11), β=105.043(9)°, V=1396.4(16)3 , Z=4, F(000)=624, Dc=1.419 g/cm3 , μ=0.105 mm1, R=0.0513 and wR=0.1246 for 14459 independent reflections (Rint=0.0647) and 2488 observed ones (I>2σ(I)). Intermolecular O-H···O and π-π stacking interactions contributed to the stability of the structure.     

A rapid, four-component synthesis of functionalized thiazoles

An efficient synthesis of 2-(dialkylamino)-4-phenyl)-1,3-thiazol-5-yl)(phenyl)methanone using acid chlorides, secondary amines, 2-bromoacethophenone and ammonium thiocyanate is described.     

含二羟基二苯酮的系列热致液晶共聚酯的合成和表征──Ⅲ．含4，4＇－二羟基二苯砜结构的共聚酯

hermotropic liquid crystalline copolyesters were synthsized from his(4-hydroxyphenyl) methanone (BHP), tereplithalic acid (TPA), p-hydroxybenzoic acid (PHB) and dihydroxydiphenyl sulfone(DPS). The properties of the copolyesters were characterized by polarized microscope with a hot stage, wide angle X-ray diffraction and differential scanning calorimetry. The results show that the copolyesters containing the BHP exhibit nematic liquid crystallinity.     

含二羟基二苯酮的系列热致液晶共聚酯的合成和表征──Ⅲ．含4，4＇－二羟基二苯砜结构的共聚酯

含二羟基二苯酮的系列热致液晶共聚酯的合成和表征──Ⅲ．含４，４＇－二羟基二苯砜结构的共聚酯董德文，池振国，倪玉山，丁孟贤（中国科学院长春应用化学研究所长春１３００２２）陈玉（东北师范大学分析测试中心长春１３００２４）关键词４，４＇－二羟基二苯酮，热致...     

A New Class of Aluminum Cations Based upon Tetradentate (N(2)O(2)) Chelating Ligands

Herein are described the synthesis and characterization of the complexes of formula LAlR (where R = Cl and L = Salen (1), SalenCl (2), Acen (3) and where R = Me and L = Salen (4), SalenCl (5), Acen (6); Salen = N,N'-ethylenebis((2-hydroxyphenyl)methylimine), SalenCl = N,N'-ethylenebis((2-hydroxy-5-chlorophenyl)methylimine), Acen = N,N'-ethylenebis((2-hydroxyphenyl)-1-ethylimine)). The LAlCl derivatives dissolve in water and MeOH to yield the cationic complexes [LAl(H(2)O)(2)](+)Cl(-) (L = Salen (7), SalenCl (8), Acen (9)) and [LAl(MeOH)(2)](+)Cl(-) (L = Salen (10), SalenCl (11), Acen (12)), respectively. An alternative preparation of the cationic species involves the reaction of the LAlCl derivative with NaBPh(4). This leads to complexes of formula [LAl(MeOH)(2)](+)BPh(4)(-) (L = Salen (13), SalenCl (14), Acen (15)). Complexes 4-6 can be reacted with either MeOH or 4-chloro-3,5-dimethylphenol (Ph') to form complexes of general formula LAlOR (R = Me, L = Salen (16), SalenCl (17), Acen (18); R = Ph', L = Salen (19), SalenCl (20), Acen (21)). All of the compounds were characterized by IR, melting points, elemental analyses, and, when soluble, NMR. Additionally, the crystal structures of 7, 13, 15, and 18 were obtained.     

Synthesis,structure and in vitro cytotoxicity testing of some 2‐aroylbenzofuran‐3‐ols

Five 2‐aroyl‐5‐bromobenzo[b]furan‐3‐ol compounds (two of which are new) and four new 2‐aroyl‐5‐iodobenzo[b]furan‐3‐ol compounds were synthesized starting from salicylic acid. The compounds were characterized by mass spectrometry and ¹H NMR and ¹³C NMR spectroscopy. Single‐crystal X‐ray diffraction studies of four compounds, namely, (5‐bromo‐3‐hydroxybenzofuran‐2‐yl)(4‐fluorophenyl)methanone, C₁₅H₈BrFO₃, (5‐bromo‐3‐hydroxybenzofuran‐2‐yl)(4‐chlorophenyl)methanone, C₁₅H₈BrClO₃, (5‐bromo‐3‐hydroxybenzofuran‐2‐yl)(4‐bromophenyl)methanone, C₁₅H₈Br₂O₃, and (4‐bromophenyl)(3‐hydroxy‐5‐iodobenzofuran‐2‐yl)methanone, C₁₅H₈BrIO₃, were also carried out. The compounds were tested for their in vitro cytotoxicity on the four human cancer cell lines KB, Hep‐G2, Lu‐1 and MCF7. Six compounds show good inhibiting abilities on Hep‐G2 cells, with IC₅₀ values of 1.39–8.03 µM.     

Synthesis of Poly(phthalazinone ether ketone) Containing Sodium Sulfonate Groups via Direct Polymerization

Poly (aryl ether ketone)s are a category of high performance engineering plastics which have outstanding thermal, physical and mechanical properties. Poly(aryl ether ketone) with sulfonic groups have received extensive attention for their potential usage as high performance gas dehumidification and ion exchange membrane materials1,2,3. Poly (phthalazinone ether ketone)4, one of poly(aryl ether ketone), shows excellent comprehensive properties and outstanding thermal stability, whose glass tra…     

Facile Synthesis of Enantiomerically Pure 1-（5-Bromo-2-chlorophenyl）-1-（4-ethoxyphenyl）ethane

A facile 7-step procedure for the synthesis of enantiomerically pure 1-（5-bromo-2-chlorophenyl）-1-（4-ethoxyphenyl）ethanes[（R）-2 and（S）-2] that started from （5-bromo-2-chlorophenyl）（4-ethoxyphenyl）methanone 3 was developed.The key step was the resolution of 2-（5-bromo-2-chlorophenyl）-2-（4-ethoxyphenyl）acetic acid 6 by crystallizations of its L-and D-menthyl esters 7 and 8 from petroleum ether to give optically pure enantiomers 9 and 10,respectively.The absolute configurations of the products were unambiguously determined by single-crystal X-ray diffractions of four key intermediates,9,10,13 and 14.This procedure is characterized by inexpensiveness,scalability and ability to produce two individual enantiomers of a diarylethane with unambiguously determined absolute configurations and high enantiomeric purities.     

热致液晶共聚酯的熔融行为及结晶结构研究

采用ＤＳＣ及ＷＡＸＤ手段对含对羟基苯甲酸热致液晶共聚酯的相变行为及结晶结构进行了初步研究。结果表明，聚合物中存在两种同属于正交晶系的不同堆积形态结晶结构，在相变上表现为双重熔融峰。     

含二羟基二苯酮系列热致液晶共聚酯的合成与表征──Ⅱ．含4，4＇－二羟基二苯酮，对苯二甲酸，对羟基苯甲酸，间苯二酚的共聚酯

采用直接熔融缩聚及固相聚合方法由４，４’－二羟基二苯酮（ＢＨＰ），对苯二甲酸（ＴＰ），对羟基苯甲酸（ＰＨＢＡ），间苯二酚（ＲＥＳ）成功地合成了四元共聚酯高分子，该聚酯的组成结构及性质由偏光显微镜、广角Ｘ－射线衍射、ＤＳＣ等手段进行表征，结果表明共聚酯具有向列型液晶特征．     

SYNTHESIS AND STRUCTURAL CHARACTERIZATION OF ZINC AND CADMIUM COORDINATION POLYMERS CONSTRUCTED BY 2-PHENYLBUTANEDIOIC ACID AND BIS(4-(1H-IMIDAZOL-1-YL)PHENYL) METHANONE LIGANDS

Journal of Structural Chemistry - Two coordination polymers [(L1)Zn(pbtda)]n (1) and [(L1)Cd(H2O)(pbtda)]n (2), (L1 = bis(4-(1H-imidazol-1-yl)phenyl)methanone,...     

Synthesis of mono- and dihalogenated derivatives of (Me2S)2B12H10 and palladium-catalyzed boron-carbon cross-coupling reactions of the iodides with grignard reagents

Two series of compounds, 9-X-1,7-(Me(2)S)(2)B(12)H(9) and 9,10-X(2)-1,7-(Me(2)S)(2)B(12)H(8) (X = Cl, Br, I), have been synthesized from reactions of 1,7-(Me(2)S)(2)B(12)H(10) with various halogenating reagents. In addition, reactions of 1,7-(Me(2)S)(2)B(12)H(10) with 2,4-(NO(2))(2)C(6)H(3)SCl and PhSeBr resulted in 9-(2',4'-(NO(2))(2)C(6)H(3)S)-1,7-(Me(2)S)(2)B(12)H(9) and 9,10-(PhSe)(2)-1,7-(Me(2)S)(2)B(12)H(8), respectively. X-ray studies of the dibromo, monoiodo, and aryl thioether derivatives show that electrophilic substitution in 1,7-(Me(2)S)(2)B(12)H(10) takes place at positions 9 and 10, as in the case of the meta-carborane 1,7-C(2)B(10)H(12). From 1,12-(Me(2)S)(2)B(12)H(10) the halides 2-X-1,12-(Me(2)S)(2)B(12)H(9) (X = Br, I) were prepared. For both 1,7- and 1,12-(Me(2)S)(2)B(12)H(10) the best iodination results were obtained using iodine monochloride in refluxing acetonitrile. In the presence of 5 mol % (PPh(3))(2)PdCl(2) the iodides 9-I-1,7-(Me(2)S)(2)B(12)H(9), 2-I-1,12-(Me(2)S)(2)B(12)H(9), and 9,10-I(2)-1,7-(Me(2)S)(2)B(12)H(8) react with RMgX (R = Me, Ph, Bn; X = Cl, Br) in THF to yield the corresponding B-alkyl- and B-aryl-substituted products in good yields without using CuI as a cocatalyst. The bromo derivative 9-Br-1,7-(Me(2)S)(2)B(12)H(9) did not react under similar conditions. No interference from the nearby Me(2)S substituent was observed in palladium-catalyzed substitution of iodide in 2-I-1,12-(Me(2)S)(2)B(12)H(9). Presumably due to the intramolecular activation of an aryl C-H bond of the benzyl substituent in the intermediate palladium complex, the yield of 9,10-Bn(2)-1,7-(Me(2)S)(2)B(12)H(8) was significantly lower than those of the dimethyl and diphenyl derivatives. The molecular structures of 9-R-1,7-(Me(2)S)(2)B(12)H(9) (R = Ph, Bn) and 2-Bn-1,12-(Me(2)S)(2)B(12)H(9) were obtained by single-crystal X-ray analysis.     

Dinuclear nickel complexes with a Ni(2)O(2) core: a structural and magnetic study

The acetylacetonate complexes [Ni(2)L(1)(acac)(MeOH)] x H(2)O, 1 x H(2)O and [Ni(2)L(3)(acac)(MeOH)] x 1.5H(2)O, 2 x 1.5H(2)O (H(3)L(1) = (2-(2-hydroxyphenyl)-1,3-bis[4-(2-hydroxyphenyl)-3-azabut-3-enyl]-1,3-imidazolidine and H(3)L(3) = (2-(5-bromo-2-hydroxyphenyl)-1,3-bis[4-(5-bromo-2-hydroxyphenyl)-3-azabut-3-enyl]-1,3-imidazolidine) were prepared and fully characterised. Their crystal structures show that they are dinuclear complexes, extended into chains by hydrogen bond interactions. These compounds were used as starting materials for the isolation of the corresponding [Ni(2)HL(x)(o-O(2)CC(6)H(4)CO(2))(H(2)O)] x n MeOH and [Ni(2)HL(x)(O(2)CCH(2)CO(2))(H(2)O)]x nH(2)O dicarboxylate complexes (x = 1, 3; n = 1-3). The crystal structures of [Ni(2)HL(1)(o-O(2)CC(6)H(4)CO(2))(H(2)O)] x MeOH, 3 x MeOH, [Ni(2)HL(3)(o-O(2)CC(6)H(4)CO(2))(H(2)O)] x 3 MeOH, 4 x 3 MeOH and [Ni(2)HL(1)(O(2)CCH(2)CO(2))(H(2)O)] x 2.5H(2)O x 0.25 MeOH x MeCN, 5 x 2.5H(2)O x 0.25 MeOH x MeCN, were solved. Complexes 3-5 show dinuclear [Ni(2)HL(x)(dicarboxylate)(H(2)O)] units, expanded through hydrogen bonds that involve carboxylate and water ligands, as well as solvate molecules. The variable temperature magnetic susceptibilities of all the complexes show an intramolecular ferromagnetic coupling between the Ni(II) ions, which is attempted to be rationalized by comparison with previous results and in the light of molecular orbital treatment. Magnetisation measurements are in accord with a S = 2 ground state in all cases.