Synthesis of 6‐Aminopropyl‐6H‐indolo[2,3‐b]quinoxaline Derivatives

A series of 6‐(3‐aminopropyl)‐6H‐indolo[2,3‐b]quinoxalines were synthesized with high yields by the reaction of 6‐(3‐chloropropyl)‐6H‐indolo[2,3‐b]quinoxaline and corresponding amines in presence of tetrabutylammonium iodide in boiling toluene or dimethylformamide at room temperature. It was found that boiling of 6‐(3‐chloropropyl)‐6H‐indolo[2,3‐b]quinoxaline in acetone with sodium iodide or in acetic acid lead to intramolecular cyclization product.     

Synthesis of tetrahydrobenzimidazo[1,2-b]quinazolin-1(2H)-one and tetrahydro-1,2,4-triazolo[5,1-b]quinazolin-8(4H)-one ring systems under solvent-free conditions

Tetraheterocyclic benzimidazo[1,2-a]quinazolin-4(1H)-one and tetrahydro-1,2,4-triazolo[5,1-b]quinazolin-8(4H)-one were synthesized in relatively high yields by the condensation reaction of an aldehyde and a cyclic beta-diketone with 2-aminobenzothiazole, 2-aminobenzimidazole or 3-amino-1,2,4-triazole without using any catalyst under solvent-free conditions.     

Syntheses of highly fluorinated 1,3,5-triazapentadienyl ligands and their use in the isolation of copper(I)-carbonyl and copper(I)-ethylene complexes

Fully fluorinated triazapentadienyl ligand [N{(C3F7)C(C6F5)N}2]- and the related [N{(C3F7)C(2-F,6-(CF3)C6H3)N}2]- have been synthesized in good yield via a convenient route and used in the isolation of three- and four-coordinate copper(I)-carbon monoxide complexes. They show fairly high nu(CO) values (>2100 cm(-1)), indicating the presence of electron-poor Cu sites. The copper(I)-ethylene adduct [N{(C3F7)C(C6F5)N}2]Cu(C2H4), featuring a three-coordinate Cu site, has also been synthesized using [N{(C3F7)C(C6F5)N}2]CuNCCH3 and C2H4.     

Extraction and Separation of Co2+ from Ni2+ Using the Novel Task-Specific Ionic Liquids of [C4H9NH3][P507]

Russian Journal of Applied Chemistry - Novel task-specific ionic liquids of [C4H9NH3][P507], [C6H13NH3][P507], [C8H17NH3][P507], [C10H21NH3][P507] and [C12H25NH3][P507] were synthesized by one-step...     

Facile one-pot synthesis of photochromic pyrans

[reaction: see text]. Photochromic pyrans, including [3H]naphtho[2,1-b]pyrans, [2H]naphtho[1,2-b]pyrans, indeno-fused naphtho[1,2-b]pyrans, and heteroannulated pyrans, were synthesized in excellent yields through a facile one-pot procedure by reaction of propargyl alcohol and naphthol or phenol derivatives in the presence of 5 mol % PPTS and 2 equiv of (MeO)3CH. Symmetrical and nonsymmetrical bispyrans can also be prepared using the protocol.     

Synthesis and in vitro evaluation of iodinated derivatives of piperazine as a new ligand for sigma receptor imaging by single photon emission computed tomography

A new series of radioiodinated analogues of 1-[2-(3,4-dimethoxyphenyl)ethyl]-4-(3-phenylpropyl)piperazine (SA4503) was synthesized and evaluated as a potential brain sigma-1 receptor imaging ligands by single photon emission computed tomography (SPECT). Iodinated analogues of SA4503 (4a-c) were prepared from piperazine in a high yield. The in vitro competition binding studies using [3H] DTG (sigma-1, 2), [3H] (+)-pentazocine (sigma-1), and [3H] DTG in the presence of carbetapentane (sigma-2) as sigma receptor selective radioligands were revealed that iodinated analogues 4a-c possess high affinities to sigma receptors (IC50: 4a=7.1, 4b=31.0, and 4c=77.3 nM). In particular, the affinity of 4a, bearing iodine at ortho position on the phenyl ring, was 4.4 times greater than SA4503, and 3 times greater than that of haloperidol. The meta-iodo analogue 4b was the same to SA4503, the lead compound. The radioiodinated derivatives, [125I] 4a, 4b were synthesized no-carrier-added from the corresponding tributyltin precursors by the iododestannylation reaction with high yields. The binding of [125I] 4a, 4b have been characterized in the rat brain membranes. These compounds were indicated single population binding to sigma receptor with high affinity (4a: Kd=1.86+/-0.34 nM, Bmax=205+/-28.9 fmol/mg protein, 4b: Kd=3.30+/-0.51 nM, Bmax=231.5+/-13.8 fmol/mg protein). In vitro blocking studies were confirmed that the high specificity of 4a, 4b. These results suggest that radioiodinated 4a and 4b are promising sigma receptors imaging ligand for pursuing further in vivo studies.     

Hydrido and chloro gallium and aluminium complexes with the tridentate bis(2-dimethylaminoethyl)amide ligand

Five-coordinate gallium and aluminium dihydrides, H2Ga[N(CH2CH2NMe2)2] () and H2Al[N(CH2CH2NMe2)2] (), were synthesized and found to be volatile and thermally stable. and reacted with H3Ga(NMe3) and H3Al(NMe3), respectively, to form H2Ga[N(CH2CH2NMe2)2]GaH3 () and H2Al[N(CH2CH2NMe2)2]AlH3 (), in which the amido nitrogen bridged between the MH2 and MH3 groups (M=Ga or Al). A mixed metal complex, H2Al[N(CH2CH2NMe2)2]GaH3 () was obtained from the reaction of with H3Al(NMe3) or with H3Ga(NMe3), and a crystal consisting of a mixture of and was structurally characterized. The five-coordinate chloro derivative, Cl2Ga[N(CH2CH2NMe2)2] (), was synthesized and characterized.     

Synthesis and electrochemical properties of 2,6-bis（6-aryl-[1,2,4]- triazolo[3,4-b][1,3,4]-thiadiazole-3-yl）pyridines

By the condensation of 2,6-bis（4-amino-5-mercapto-[1,2,4]-triazoles-2）pyridine with aromatic acid in the presence of phosphorus oxychloride. Compounds of 2,6-bis（6-aryl-[1,2,4]-triazolo[3,4-b][1,3,4]-thiadiazole-3-yl）pyridines were synthesized. Their structures were confirmed by IR, ^1H NMR spectroscopies and elemental analysis. Their electrochemical behavior and cyclic voltammogram also were be studied. The results showed that they have high ionization potentials and good affinity.     

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.     

Eta 1 and eta 2 Coordination of 1-amino-closo-dodecaborate

The reaction of the sodium salt of 1-amino-closo-dodecaborate [Na]2[NH2-B12H11] ([Na]2[1]) with [Au(PPh3)Cl] and [Ni(THF)2(Br)2] led to eta 1(N) coordination of 1in [Na][Au(PPh3)(NH2-B12H11)] (2) and [Na]6[Ni(NH2-B12H11)4] (3), respectively. Furthermore, eta 2(N,BH) coordination of was found in [MePPh3][Rh(PPh3)2(NH2-B12H11)] (4), which was synthesized by the reaction of [MePPh3][Na][1] with [Rh(PPh3)3Cl]. All compounds were characterized by single crystal X-ray diffraction and heteronuclear NMR spectroscopy.     

Synthesis of nitrosylruthenium complexes containing 2,2':6',2"-terpyridine by reactions of alkoxo complexes with acids

Nitrosylruthenium complexes containing 2,2':6',2"-terpyridine (terpy) have been synthesized and characterized. The three alkoxo complexes trans-(NO, OCH3), cis-(Cl, OCH3)-[RuCl(OCH3)(NO)(terpy)]PF6 ([2]PF6), trans-(NO, OC2H5), cis-(Cl, OC2H5)-[RuCl(OC2H5)(NO)(terpy)]PF6 ([3]PF6), and [RuCl(OC3H7)(NO)(terpy)]PF6 ([4]PF6) were synthesized by reactions of trans-(Cl, Cl), cis-(NO, Cl)-[RuCl2(NO)(terpy)]PF6 ([1]PF6) with NaOCH3 in CH3OH, C2H5OH, and C3H7OH, respectively. Reactions of [3]PF6 with an acid such as hydrochloric acid and trifluoromethansulforic acid afford nitrosyl complexes in which the alkoxo ligand is substituted. The geometrical isomer of [1]PF6, trans-(NO, Cl), cis-(Cl, Cl)-[RuCl2(NO)(terpy)]PF6 ([5]PF6), was obtained by the reaction of [3]PF6 in a hydrochloric acid solution. Reaction of [3]PF6 with trifluoromethansulforic acid in CH3CN gave trans-(NO, Cl), cis-(CH3CN, Cl)-[RuCl(CH3CN)(NO)(terpy)]2+ ([6]2+) under refluxing conditions. The structures of [3]PF6, [4]PF6.CH3CN, [5]CF3SO3, and [6](PF6)2 were determined by X-ray crystallograpy.     

无胺合成[Fe]ZSM-5分子筛的结构鉴定及其催化性能的研究

不用有机胺为模板剂,在碱性介质中采用水热合成法成功地合成了[Fe]ZSM-5分子筛.用X射线衍射、透射电镜、红外光谱、顺磁共振谱、X射线光电子能谱和穆斯堡尔谱等对其结构进行了表征,结果表明,Fe原子进入了分子筛骨架,并处于四面体的配位环境.在由甲醇转化为汽油的过程中,以本文合成的[Fe]ZSM-5与用有机胺为模板剂合成的[Fe]ZSM-5分子筛为催化剂相比,其活性和选择性几乎相同,且都比通常的H[Al]ZSM-5好,C₅组分以上的选择性大于80%,且芳烃(包括脂环烃)和异构烃的含量达75%以上.     

Tetravalent Platinum Complexes: Synthesis,Structure, and Antimicrobial Activity

The complexes [(C2H5)2NH2]2[PtCl6], [(C2H5)4N]2[PtCl6], and [(CH3)3NH]2[PtCl6] were prepared by the reaction of hexachloroplatinic acid with organylammonium chlorides in acetonitrile. Structure of these compounds was determined by X-ray analysis and infrared spectroscopy. The synthesized crystals consist of tetrahedral organylammonium cations and hexachloroplatinate octahedral anions. The antimicrobial activity of the synthesized complexes against the Escherichia coli strain M-17 was studied.     

Chlorine anion encapsulation by molecular capsules based on cucurbit[5]uril and decamethylcucurbit[5]uril

Three barrel-shaped artificial molecular capsules 1-3, based on normal cucurbit[5]uril (Q[5]) and decamethylcucurbit[5]uril (Me10Q[5]), were synthesized and structurally characterized by single-crystal X-ray diffraction. Encapsulation of a chlorine anion in the cavity of a Q[5] or Me10Q[5] to form closed a molecular capsule with the coordinated metal ions or coordinated metal ions and water molecules in the crystal structures of these compounds is common. The three complexes [Pr2(C30H30N20O10)Cl3(H2O)13]3+ 3 Cl- x 5 H2O (1), [Sr2(C40H50N20O10)(H2O)4Cl]3+ 3 Cl- x 2 (HCl) 19 H2O (2) and [K(C40H50N20O10)(H2O)Cl] x [Zn(H2O)2Cl2] x [ZnCl4]2- x 2 (H3O)+ x 8 H2O (3) all crystallize as isolated molecular capsules.     

Synthesis of New Benzoxazinone,Quinazolinone, and Pyrazoloquinazolinone Derivatives and Evaluation of Their Cytotoxic Activity Against Human Breast Cancer Cells

Synthesis of 2‐[3‐(3,4‐dichlorophenyl)‐3‐oxoprop‐1‐enyl]‐4H‐benzo[3,1]oxazin‐4‐one 2 as a precursor to synthesize quinazolinones 5 , 7 pyrazolylquinazolinones, 4 , 12 , 13 , 14 , 16 benzothiazine thione 10 , benzene derivative 3 pyrroloquinazolinone 6 , benzoimidazoquinazolinone 8 , and pyrazolotriazepinoquinazolinone 15 . The structures of the newly synthesized compounds were established by their elemental analyses and spectral data. Most of the synthesized compounds exhibited high antitumor and cytotoxic activity against human breast cancer cells.     

Bisindoles. 38. Synthesis of Some Derivatives of 1H,6H-Indolo[7,6-g]indole

1H,6H,2,3,7,8-Tetramethylindolo[7,6-g]indole and 1H,8H,2,3,4,5,9,10,11,12-octahydrocarbazolo[3,2-c]carbazole were synthesized by the condensation of 1,5-naphthylenedihydrazine with alkyl ketones followed by cyclization of the obtained hydrazones without isolation. The respective N,N-dibenzyl derivatives were obtained by benzylation of the alkyl-substituted compounds. A new spirocyclic system was synthesized by nucleophilic addition of 2,3,3,7,8,8-hexamethylindolenino[7,6-g]indolenine to 2',3'-dimethoxycarbonylspirofluorenecyclopropene.     

Synthesis of Novel Benzisothiazolone Derivatives as Potential Antifoulants

Novel antifoulant 2‐(3‐oxobenzo[d]isothiazol‐2(3H)‐yl)acetohydrazide (2) and 3‐oxobenzo[d]isothiazol‐2(3H)‐yl acetic acid [1‐phenylmethylidene]‐hydrazides (3a–3h) were synthesized in good yields, and their structures were characterized by means of UV, IR, ¹H NMR, MS, and elemental analysis.     

Synthesis and characterization of ethylbis(2-pyridylethyl)amineruthenium complexes and two different types of C-H bond cleavage at an ethylene arm

Ruthenium complexes bearing ethylbis(2-pyridylethyl)amine (ebpea), which has flexible -C(2)H(4)- arms between the amine and the pyridyl groups and coordinates to a metal center in facial and meridional modes, have been synthesized and characterized. Three trichloro complexes, fac-[Ru(III)Cl(3)(ebpea)] (fac-[1]), mer-[Ru(III)Cl(3)(ebpea)] (mer-[1]), and mer-[Ru(II)Cl(3){η(2)-N(C(2)H(5))(C(2)H(4)py)═CH-CH(2)py}] (mer-[2]), were synthesized using the Ru blue solution. Formation of mer-[2] proceeded via a C-H activation of the CH(2) group next to the amine nitrogen atom of the ethylene arm. Reduction reactions of fac- and mer-[1] afforded a triacetonitrile complex mer-[Ru(II)(CH(3)CN)(3)(ebpea)](PF(6))(2) (mer-[3](PF(6))(2)). Five nitrosyl complexes fac-[RuX(2)(NO)(ebpea)]PF(6) (X = Cl for fac-[4]PF(6); X = ONO(2) for fac-[5]PF(6)) and mer-[RuXY(NO)(ebpea)]PF(6) (X = Cl, Y = Cl for mer-[4]PF(6); X = Cl, Y = CH(3)O for mer-[6]PF(6); X = Cl, Y = OH for mer-[7]PF(6)) were synthesized and characterized by X-ray crystallography. A reaction of mer-[2] in H(2)O-C(2)H(5)OH at room temperature afforded mer-[1]. Oxidation of C(2)H(5)OH in H(2)O-C(2)H(5)OH and i-C(3)H(7)OH in H(2)O-i-C(3)H(7)OH to acetaldehyde and acetone by mer-[2] under stirring at room temperature occurred with formation of mer-[1]. Alternative C-H activation of the CH(2) group occurred next to the pyridyl group, and formation of a C-N bond between the CH moiety and the nitrosyl ligand afforded a nitroso complex [Ru(II)(N(3))(2){N(O)CH(py)CH(2)N(C(2)H(5))C(2)H(4)py}] ([8]) in reactions of nitrosyl complexes with sodium azide in methanol, and reaction of [8] with hydrochloric acid afforded a corresponding chloronitroso complex [Ru(II)Cl(2){N(O)CH(py)CH(2)N(C(2)H(5))C(2)H(4)py}] ([9]).     

Synthesis,Bioactivity and Crystal Structure Analysis of Novel Benzo[d]isothiazol-3（2H）-ones

Two compounds,3-oxo-N-o-tolylbenzo[d]isothiazole-2(3H)-carboxamide (1) and N-(2-methoxyphenyl)-3-oxobenzo[d]isothiazole-2(3H)-carboxamide (2),were synthesized from the initial compound benzo[d]isothiazol-3(2H)-one (BIT) and characterized by 1 H NMR,IR and elemental analysis,respectively.The single crystals of compounds 1 and 2 were obtained and determined by X-ray diffraction analysis.The preliminary results of biological activity experiment show that some of the title compounds exhibited a favorable antimicrobial activity.     

The first example of solvothermally synthesized thioantimonates(V) with ethylenediamine coordinated lanthanide(III): [Sm(en)4]SbS4 x 0.5en and [Sm(en)3(H2O)(micro-SbS4)]infinity

Under mild solvothermal conditions two novel thioantimonates(V) [Sm(en)4]SbS4 x 0.5en (1) and [Sm(en)3(H2O)(micro-SbS4)]infinity (2) were synthesized; the structure of 1 contains discrete [Sm(en)4]3+ and [SbS4]3 ions, while 2 consists of neutral [Sm(en)3(H2O) (micro-SbS4)] one-dimensional chains.