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1.
Abstract Novel thio- and alkoxy-substituted benzoquinone derivatives were synthesized from the reactions of p-chloranil (1) and related nucleophiles in a sodium carbonate (Na 2CO 3) solution of acetonitrile or in chloroform with Et 3N. The structures of novel compounds were characterized by using microanalysis, FTIR, 1H NMR, 13C NMR, MS, CV, and fluorescence spectroscopy. [Supplementary materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements for the following free supplemental files: Additional text and figures.] 相似文献
2.
The vanadium(III) complexes, V(S 2CNMe 2) 3 ( 1) and V(S 2CN i Pr 2) 3 ( 2) were prepared and characterized by analysis, IR, electronic and 1H NMR spectra. The complexes show reversible thermochromic behaviour. MM2 calculations were used to simulate the molecular structure of 1. For 2, variable temperature 1H NMR revealed hindered rotation about C–N bonds. The rotational energy barrier (38?kJ?mol ?1) was obtained by molecular mechanics force-field calculations. 相似文献
3.
The triorganotin(IV) complex Ph 3Sn(OPhMe-2) ( 1) has been synthesized by the reaction of Ph 3SnCl with NaOPhMe-2, while complexes of composition n-Bu 3Sn(OPhMe-2) ( 2) and Me 3Sn(OPhMe-2) ( 3) (where ?OPhMe-2 = ?OC 6H 4CH 3-2) have been obtained from the reaction of n-Bu 3SnCl and Me 3SnCl with 2-methylphenol in the presence of triethylamine in carbon tetrachloride. The complexes have been characterized by elemental analyses, molar conductance measurements, molecular weight determination, and IR, 1H NMR, 13C NMR, and mass spectral studies. Thermal behavior of the complexes has been studied by TG and DTA techniques. The organotin(IV) complexes have also been screened for antibacterial activity and exhibit appreciable activity. The reactions of the complexes with 3- and 4-cyanopyridines yielded 1 : 1 adducts authenticated by physicochemical and IR and 1H NMR spectral data. 相似文献
4.
o-Dihydroxy-4-(3,4-dimethoxyphenyl)-chromenones (coumarins; 3a, b) were synthesised from 1,2,3-trihydroxy- or 1,2,4-triacetoxybenzenes through a reaction with ethyl 3-(3,4-dimethoxyphenyl)-3-oxopropanoate in H 2SO 4 or CF 3COOH. The chromenone-crown ethers ( 4a– f) were prepared from the cyclic condensation of o-dihydroxy-4-(3,4-dimethoxyphenyl)chromenones ( 3a, b) with poly(ethylene glycol) ditosylates, in the presence of CH 3CN/alkali carbonates. The chromatographically purified original chromenone-crown ethers were identified by 1H NMR, 13C NMR, MALDI-TOF mass spectrometry and elemental analysis. The 1:1 binding constants of Li +, Na + and K + with the chromenone-crown ethers were estimated in acetonitrile using fluorescence emission spectroscopy. The complexing-enhanced fluorescence spectra and complexing-enhanced quenching fluorescence spectra, along with the cationic recognition rules of the crown ethers allowed the ion binding powers to be determined. 相似文献
5.
Three new propanedithiolate-type iron–sulfur complexes containing tris(aromatic)phosphine ligands, [{( μ-SCH 2) 2CH 2}Fe 2(CO) 5L] (L?=?P(PhOMe- p) 3, 1; P(PhMe- p) 3, 2; P(PhF- p) 3, 3), have been prepared through carbonyl substitution in the presence of Me 3NO. The new complexes 1–3 were characterized by elemental analysis, IR, 1H, 13C{ 1H}, and 31P{H} NMR spectra. The molecular structures of 1–3 were unequivocally determined by single crystal X-ray diffraction, in which the tris(aromatic)phosphine coordinated to Fe resides in an apical position of the pseudo-square-pyramidal geometry. IR spectroscopy and X-ray crystallographic analysis for 1–3 have indicated that the highly electron rich tris(aromatic)phosphine ligands (where the corresponding electron-donating abilities display the following order of P(PhOMe- p) 3?>?P(PhMe- p) 3?>?P(PhF- p) 3) result in a considerable red shift of the CO-stretching frequencies and a clear change of the Fe–Fe bond distances in 1–3. 相似文献
6.
The novel monosubstituted benzoquinone compounds 3e , 3g , 3h ; 2,5‐ O‐ substituted benzoquinone compounds 4a , 4b , 4c , 4d , 4e 4g and known compound 4h and 2,6‐ O‐ substituted benzoquinone compounds 5e , 5f , 5g , 5h were obtained by the reaction of p‐chloranil ( 1 ) and related alcohol compounds in potassium carbonate (K 2CO 3) solution of acetonitrile or chloroform with Et 3N. The novel cyclic compounds 7 , 8 and 10 , 11 were obtained from the reaction of p‐chloranil ( 1 ) and diols in potassium carbonate (K 2CO 3) solution of acetonitrile at room temperature. The structures of novel compounds were characterized by using micro analysis, FT‐IR, 1H‐NMR, 13C‐NMR, MS and cyclic voltammetry. 相似文献
7.
AbstractKetene dithioacetal mediated chemo- and regioselective synthesis of a series of novel 1,3,4,5-tetrasubstituted pyrazole derivatives ( 4a-l) integrated with a bioactive indole nucleus was achieved by reacting substituted 2-(1-methyl-1H-indole-3-carbonyl)-3,3-bis-(methylthio)-acrylonitrile ( 2) and substituted phenyl hydrazine hydrochloride ( 3) in the presence of a catalytic amount of anhydrous K 2CO 3 under reflux conditions. The structures were ascertained by 1H NMR, NOESY, 13C NMR, FT-IR, and HRMS data. In vitro cytotoxicity evaluation of the synthesized compounds against MCF 7 (breast carcinoma) and normal Vero (monkey kidney) cell lines revealed that the compound 5-(5-Bromo-1-methyl-1 H-indol-3-yl)-1-(4-cyano-phenyl)-3-methylsulfanyl-1 H-pyrazole-4-carbonitrile ( 4k) showed significant cytotoxicity against MCF 7 (GI 50 = 15.6 µM) with low cytotoxicity against normal Vero cell line. Most of the synthesized compounds were also found to possess excellent anti-inflammatory and antioxidant (DPPH, NO, H 2O 2 and SOR) potential. 相似文献
8.
以3-硝基邻苯二甲腈为起始原料, 与正戊醇反应合成3-戊氧基邻苯二甲腈( 1), 然后在高温溶剂1-氯萘中经缩聚反应合成二氯-轴向取代-四- α-(3-戊氧基)锡酞菁( 2), 2进一步与2-羟基吡啶在 N, N-二甲基甲酰胺中合成二-吡啶氧基-轴向取代-四- α-(3-戊氧基)锡酞菁配合物 3, 同时对相关化合物分别进行了元素分析, IR, 1H NMR, UV/Vis, 荧光和质谱表征. 相似文献
9.
Reactions of HgX 2 (X?=?Cl, N 3, NO 3) with ( E)-2-methoxy-N-(pyridin-2-ylmethylene)aniline (L 1) and ( E)-4-methoxy-N-(pyridin-2-ylmethylene)aniline (L 2) in ethanol gave two monomers, [HgL 1(Cl) 2] ( 1) and [HgL 2(NO 3) 2(DMSO)] ( 5), and three coordination polymers, {[HgL 1(N 3) 2] 2·Hg(N 3) 2} n ( 2), [HgL 2(Cl) 2] n ( 3), and [HgL 2(NO 3) 2] n·nCH 3CN ( 4). Compounds 1–5 were characterized by elemental analysis, IR, NMR spectroscopy, and single-crystal X-ray diffraction. The common feature of monomeric 1 and 5 is the presence of intra- and intermolecular Hg–O bonds. In the absence of these, polymeric structures arise as a result of azide, chloride, and nitrate bridging in 2, 3, and 4, respectively. Fluorescent properties of 1–5 were also investigated. 相似文献
10.
Reaction of [Pd(dppe)Cl 2/Br 2] with AgOTf in a dichloromethane medium followed by ligand addition led to [Pd(dppe)(OSO 2CF 3) 2] and then [Pd(dppe)(RaaiR)](OSO 2CF 3) 2 [RaaiR′ = p-R-C 6H 4-N=N-C 3H 2-NN-1-R′, ( 1–3), abbreviated as a N,N′-chelator, where N(imidazole) and N(azo) are represented by N and N′, respectively; R = H ( a), Me ( b), Cl ( c) and R′ = Me ( 1), CH 2CH 3 ( 2), CH 2Ph ( 3), OSO 2CF 3 is the triflate anion, dppe = 1,2-bis-(diphenylphosphinoethane)]. 31P “ 1H” NMR confirmed that due to the two phosphorus atom interaction in the azoimine symmetrical environment one sharp peak was
formed. The 1H NMR spectral measurements suggest that azo-imine link with lot of phenyl protons in the aromatic region. 13C ( 1H) NMR spectrum, 1H, 1H COSY and 1H, 13C HMQC spectrum assign the solution structure and stereo-retentive conformation in each complex. 相似文献
11.
5-HT 3 receptor antagonists, such as Ondansetron, are used for anti-emesis after chemotherapy, radiotherapy and operations. Some
Ondansetron analogs possessing piperazine ring as side chains were synthesized in our lab. Thus, one of the two carbonyl groups
of starting material 1,3-cyclohexandione ( 1) was condensed with phenylhydrazine hydrochloride to form monophenylhydrazone ( 2). 1,2,3,9-Tetrahydro-4 H-carbazol-4-one ( 3) was prepared from 2
via cyclization and rearranged in the presence of ZnCl 2. Through a methylation reaction, compound 3 was converted to 1,2,3,9-tetrahydro-9-methyl-4 H-carbazol-4-one ( 4). 3-Dimethylaminomethyl substituted compound ( 5) was synthesized from 4 by a Mannich reaction in glacial acetic acid. Nine novel 1,2,3,9-tetrahydro-9-methyl-3-(4-substituted-piperazin-1-ylmethyl)-4 H-carbazol-4-one derivatives ( 6a–6i) were synthesized through nucleophilic substitution reaction of 5 with piperazines. The structures of all the target compounds were determined by elemental analysis, IR, MS, 1H NMR and 13C NMR spectra. The results of preliminary pharmacological test show that part of the novel compounds have antiemetic activity
comparable to that of the control Ondansetron.
__________
Translated from Chinese Journal of Organic Chemistry, 2008, 28(2) (in Chinese) 相似文献
12.
芳甲酰肼和氯乙酸在二甲苯中反应生成了一系列的2-芳基-5-氯甲基-1,3,4-噁二唑( 1a~ 1j), 继而与2-(2-三氟甲基苯并咪唑-1-亚甲基)-5-巯基-1,3,4-噁二唑( 2)在乙醇-水的溶液中反应得到了一系列的含2-三氟甲基苯并咪唑的双噁二唑硫醚 3a~ 3j, 再用硝酸氧化得到相应的亚砜衍生物 4a~ 4j. 化合物的结构经元素分析, IR, 1H NMR确证. 相似文献
13.
Reactions of copper(I) halides with triphenyl phosphine in acetonitrile followed by the addition of salicylaldehyde N-ethylthiosemicarbazone {(2-OH–C 6H 4)(H)C 2=N 3–N 2H–C 1(=S)N 1HEt, H 2stsc-NEt} in chloroform in 1?:?2?:?1 (Cl) or 1?:?1?:?1 (Br, I) molar ratios yield mononuclear, [CuCl( η 1-S-H 2stsc-NHEt)(PPh 3) 2] ( 1) and sulfur-bridged dinuclear, [Cu 2X 2( μ-S-H 2stsc-NEt) 2(PPh 3) 2] (X?=?Br, 4; I, 5) complexes. Similarly, reaction of silver halides (Cl, Br) with H 2stsc-NEt in acetonitrile followed by the addition of PPh 3 to the solid that formed (1?:?1?:?2 molar ratio), yielding mononuclear complexes, [AgX( η 1-S-H 2stsc-NHEt)(PPh 3) 2] (Cl, 2; Br, 3). All these complexes are characterized with analytical data, IR, and NMR spectroscopy and single-crystal X-ray crystallography. The ligand favored η 1-S bonding in 1, 2, and 3, and μ-S bonding in 4 and 5. Cu?···?Cu contacts were 3.063?Å. The complexes form 1-D or 2-D H-bonded networks, entrapping solvent in some cases. 相似文献
14.
Functionalized bis(amino)phosphines of the type PhP(NHR) 2 ( 1a–c ) and aminophosphines of the type Ph 2PNHR ( 2a–c ) have been synthesized by treating PhPCl 2 or Ph 2PCl with corresponding primary amines of H 2N-R where R = -CH 2SO 3H, -C 6H 4SO 3H, and benzo-15-crown-5. The molybdenum(0) complex of the aminophosphine ( 3 ) has been obtained by reacting cis-[Mo(CO) 4(bipy)] with aminophosphine ( 2c ). The synthesized aminophosphines, bis(amino)phosphines, and the molybdenum(0) complex have been characterized by IR, 1H NMR, 31P NMR, and MS spectroscopic techniques and by elemental analysis. 相似文献
15.
[Ru(CO)(PPh 3) 2(η 3- O,N3,S-TSC 1)] ( 1), [Ru(Cl)(CO)(PPh 3) 2(η 2- N3,S-TSC 2)] ( 2), and [Ru(Cl)(CO)(PPh 3) 2(η 2- N3,S-TSC 3)] ( 3) have been prepared by reacting [Ru(H)(Cl)(CO)(PPh 3) 3] with the respective thiosemicarbazones TSC 1 ( 2- hydroxy- 3- methoxybenzaldehyde thiosemicarbazone), TSC 2 ( 3- hydroxybenzaldehyde thiosemicarbazone), and TSC 3 ( 3,4- dihydroxybenzaldehyde thiosemicarbazone) in a 1?:?1 M ratio in toluene and all of the complexes have been characterized by UV–vis, FT-IR, and 1H and 31P NMR spectroscopy. The spectroscopic studies showed that TSC 1 is coordinated to the central metal as a tridendate ligand coordinating via the azomethine nitrogen (C=N), phenolic oxygen, and sulfur to ruthenium in 1, whereas TSC 2 and TSC 3 are coordinated to ruthenium as a bidentate ligand through azomethine nitrogen (C=N) and sulfur in 2 and 3. Oxygen sensitivities of 1–3 and [Ru(Cl)(CO)(PPh 3) 2(η 2- N3,S-TSC 4)] ( 4), and antimicrobial activities of 1–3 have been determined. 相似文献
16.
Zn(II) complexes of N-(quinolin-8-yl)picolinamide (HL1) (1) and N2,N6-di(quinolin-8-yl)pyridine-2,6-dicarboxamide (H2L2) (2) have been synthesized by deprotonation of the ligands and characterized by IR, NMR, and Single crystal X-ray crystallography. The mononuclear [Zn(L1)2] (3) and homodinuclear [Zn2(L2)2] (4) complexes are characterized by distorted octahedral geometries stabilized by hydrogen bonding and weak π···π interaction. The complexes demonstrate intense fluorescence bands in comparison with their corresponding ligands with well-distinguished intensity. The complexes act as efficient catalysts in various transesterification reactions. Among those, the best results have been achieved with complex 3 in conversion of 4-nitrophenylacetate into methyl acetate within 3 h. 相似文献
17.
Octachlorocyclotetraphosphazene, N 4P 4Cl 8, ( 1) was reacted with N, N′-dibenzylethylenediamine to synthesize partially substituted monospiro- ( 2), dispiro- ( 5) and tetraspirocyclotetraphosphazene ( 8) derivatives. The reactions of 2 and 5 with excess pyrrolidine and morpholine produced fully substituted pyrrolidino ( 3 and 6) and morpholino ( 4 and 7) spirocyclotetraphosphazenes. The structures of the compounds were determined with 1D ( 1H, 13C, 31P, and DEPT) NMR, 2D (HSQC) NMR, ESI-MS, FTIR, and elemental analysis. The solid-state structures of 6 and 7 were examined by X-ray crystallography. In 7, intramolecular C-H…O hydrogen bonds link the molecules into centrosymmetric dimmers. The cytotoxic activity of all the compounds against human cervix carcinoma cell lines (HeLa) was investigated. The study showed that these compounds exert limited cytotoxic, apoptotic and necrotic effects on HeLa cancer cell lines. 相似文献
18.
Dehydrohalogenation and metallation of boranato-bis-trimethylphosphonium salts ( 1), using two equivalents of a lithiumalkyl in tetrahydrofuran, leads to a solvated organolithium reagent H 2B[(CH 3) 2PCH 2] 2Li ( 3) which can be converted into a 1:1n1-complex with tetramethylethylenediamin ( 4). 3 reacts with anhydrous metal(II) halides to form spirocyclic coordination compounds of the type H 2B[(CH 3) 2PCH 2] 2
M[CH 2P(CH 3) 2] 2BH 2 ( 5–9, M=Be, Mg, Zn, Cd, Hg). The reaction of [(CH 3) 3PBH 2P(CH 3) 3]Br ( 1) with lithium tetramethylmetalates Li[ M(CH 3) 4], M=Al, Ga, on heating in the absence of a solvent affords the metallocycles H 2B[(CH 3) 2PCH 2] 2
M(CH 3) 2 ( 10, 11) with evolution of methane. The products can be sublimed from the reaction mixture. The proposed structures of the new compounds, with tetrahedrally coordinated central atoms and strong covalent metal-carbon interactions, are supported by mass, IR and 1H, 7Li, 11B, 13C, and 31P NMR spectra. Compound 9 represents a rare case of a tetracoordinate organomercurial, compound 5 is the first nonionic tetraalkylberyllate. 相似文献
19.
Reaction of RuCl 2(PPh 3) 3with pyrimidine-2-thione (HpymS) in a 1:2?mol ratio in dry benzene in the presence of triethylamine as base yielded a complex of stoichiometry [Ru(pymS) 2(PPh 3) 2] ( 1). This has been characterized using analytical data and IR, 1H, 13C and 31P NMR spectroscopy. 1H NMR confirmed the deprotonation of HpymS. 31P NMR spectra showed a single peak confirming equivalent P atoms. Complex 1 crystallizes in space group Pī and HpymS acts as a η 2- N, S-deprotonated bidentate anionic ligand. The coordination geometry around the Ru center is distorted octahedral with cis dispositions of P atoms, as well as two N atoms of pymS – and trans S atoms of pymS –. Important bond distances and angles are: Ru–N, 2.119(2), 2.106(2); Ru–S, 2.4256(8), 2.4413(8); and Ru–P, 2.3266(7), 2.3167(7)?Å; P(2)–Ru(1)–P(1), 96.07(3); N(21)–Ru(1)–N(11), 83.46(9); and S(1)–Ru(1)–S(2), 153.02(3)°. 相似文献
20.
The novel substituted 2,3-dichloro-1,4-naphthoquinone derivatives were synthesized from the reactions of ( 1) and related nucleophilles in sodium carbonate (Na 2CO 3) solution of ethanol, chloroform with Et 3N, or potassium carbonate (K 2CO 3) solution of acetonitrile. The structures of novel compounds were characterized by using microanalysis, Fourier transform–infrared, 1H NMR, 13C NMR, mass spectrometry, and cyclic voltammetry (CV). [Supplementary materials are available for this article. Go to the publisher's online edition of Synthetic Communications® for the following free supplemental resource(s): Full experimental and spectral details.] 相似文献
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