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1.
Syntheses of 2,5-bis(4-methyl-2-thienyl)thiophene 3 and 2,5-bis(4-methyl-2-thienyl)pyrrole 4 are described. The key step involves Stetter reaction between 4-methyl-2-thiophenecarboxaldehyde and divinyl sulfone. Cyclizaton of the resulting 1,4-bis-(4-methyl-2-thienyl)-1,4-butanedione 2 with Lawesson's reagent gives 2,5-bis(4-methyl-2-thienyl)thiophene 3, whereas condensation with ammonium acetate provides the 2,5-bis(4-methyl-2-thienyl)pyrrole 4. 相似文献
2.
A new ternary ion-association complex of tungsten(VI), 4-nitrocatechol (NC), and 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium
bromide (Thiazolyl Blue, MTT) was obtained and studied using an extraction-spectrophotometric method. The optimum pH, reagent
concentrations, and extraction time were determined. The composition of the complex was found to be W(VI): NC: MTT = 1: 2:
2. The extraction process was investigated quantitatively and the key constants were calculated. The molar absorptivity of
the chloroform extract at λmax = 415 nm was 2.8 × 104 dm3 mol−1 cm−1, and the Beer’s law was obeyed up to 8.8 μg cm−3 tungsten(IV). The limit of detection and limit of quantification were calculated to be 0.27 μg cm−3 and 0.92 μg cm−3, respectively. The effect of foreign ions and reagents was studied and a competitive method for determination of tungsten
in products from ferrous metallurgy was developed. The residual standard deviation and the relative error were 0.53 % and
0.2 %, respectively. 相似文献
3.
二(2,4,4—三甲基戊基)膦酸从盐酸介质中萃取钍(Ⅳ)的机理 总被引:1,自引:0,他引:1
研究了二(2,4,4-三甲基戊基)膦酸的正辛烷溶液从盐酸介质中萃取钍的机理。在未控制离子强度下,萃取平衡反应为:Th^4++Cl^-+3(HA)2(o)→ThClA3(HA)3(o)+3H^+。在控制离子强度为1.0mol/L时,萃取反应为Th^4++2Cl^-+3(HA)2(O)→ThCl2A2.(HA)4(P)+2H^+。用饮和法确定的萃合物组成为ThClA3.计算了萃取反应的平衡常数及热力学 相似文献
4.
(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. 相似文献
5.
Sodium Oxonitridometallates(VI) of Molybdenum and Tungsten, Na4MO2N2 (M = Mo, W) MoO3 as well as WO3 react with an excess of NaNH2 in autoclaves at temperatures ranging from 250°C to 750°C to yield – in contrast to Ta2O5 [1] – oxonitridometallates of general composition Na4MX4 and other products like Na5WO4N [2]. The compounds decompose in moist air within minutes to Na2WO4, Na2MoO4 and Na2MoO4 · xH2O, respectively. The structures of the Na4MX4 phases were determined from single crystal X-ray diffraction data. They crystallize triclinic in the Na4CoO4-type structure [3] P1 , Z = 2 with the following cell constants: 相似文献
6.
Roland Lang Arno Schrwerth Kurt Polborn Walter Ponikwar Wolfgang Beck Theodor Severin Kay Severin 《无机化学与普通化学杂志》1999,625(8):1384-1390
Organometallic Compounds with N -substituted 3-Hydroxy-2-methyl-4-pyridone Ligands: square planar Rhodium(I), Iridium(I), and Palladium(II) Complexes Reactions of [(OC)2MCl]2 (M = Rh, Ir) or [(cod)RhCl]2 with the anions of N-Aryl or N-Alkyl substituted 3-hydroxy-2-methyl-4-pyridones (O–O′) yield complexes of the general formula [L2M(O–O′)]. Compounds of this type are also available from reactions of [(OC)2Rh(acac)] with the corresponding neutral ligands. Substitution of one carbonyl-ligand of the N-phenyl complex [(OC)2Rh(C12H10NO2)] ( 2 ) with cyclooctene affords [(OC)(C8H14)Rh(C12H10NO2)] ( 8 ). The palladium complexes [(R3P)Pd(O–O′)Cl] (R = Et, Bu), [(C6H4CH2NMe2) · Pd(O–O′)] and [(Et3P)2Pd(O–O′)]BF4 ( 9 – 12 ) were synthesized from [(R3P)PdCl2]2, [(C6H4CH2NMe2)PdCl]2 or [(Et3P)PdCl2]. The structures of the N-methyl compounds [(OC)2Rh(C7H8NO2)] ( 1 ) and [(Ph3P)Pd(C7H8NO2)Cl] ( 9 ) were determined by single crystal X-ray diffraction. 相似文献
7.
Rapid Solvent Extraction of Tin(IV) with High Molecular Weight Amine from Hydrochloric Acid Solution
A novel method has been developed for the solvent extraction of tin(IV) from 8 M hydrochloric acid with 4% N‐n‐octylaniline. Tin(IV) from the organic phase was determined spectrophotometrically with pyrocatechol violet at 550 nm. Extraction was found to be quantitative in the range of 7–10 M hydrochloric acid. When the concentration of N‐n‐octylaniline was varied from 0.05–20% in xylene, it showed that optimum concentration was > 3%. Amongst diluents like benzene and xylene, toluene was found to be an effective diluent. Effect of shaking time, concentration of metal ion, and salting out agents was studied. Tolerance limits of various diverse ions were determined by masking interfering cations. Tin(IV) was separated from associated elements in its binary mixture with Se(IV), Sb(III), Bi(III), Pb(II), Au(III), Cu(II) and Zn(II) and from its ternary mixtures with Sb(III), Bi(III) and Cu(II), Au(III). The proposed method was applied for separation and determination of tin(IV) in tin bearing alloys and foodstuffs. 相似文献
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10.
The reaction of 2-amino-4-methyl-6-(2-pyridyl)-7,8-dihydroindazolo[4,5-d]thiazole, obtained by treating 3-methyl-4-oxo-1-(2-pyridyl)-4,5,6,7-tetrahydroindazole with pyridinium bromide perbromide and then with thiourea, and 2-amino-4-methyl-6-phenyl-7,8-dihydroindazolo[4,5-d]thiazole with 4-bromo-, 4-fluoro-, 4-dimethylamino-, 4-methoxy-, 3,4-dimethoxy-, and 3,4-methylenedioxybenzaldehydes, furfural, pyridinecarbaldehyde, and thiophenecarbaldehyde gave the corresponding Schiff bases. The products of the condensation of these aminothiazoles with cinnamaldehyde, 1-(2-pyridyl)- and 4-chloro-1-(2,4-difluorophenyl)-5-formyl-3-methyl-6,7-dihydroindazoles, 2-formyl-dimedone, and 2-formyl-1,3-indanedione were also obtained. 相似文献
11.
12.
Sorption and volume dilation isotherms of semicrystalline poly(4-methyl-1-pentene) (PMP) were measured using CO2 and C3H8 as penetrants, which have sieving diameters of 3.3 and 4.3 Å, respectively. On the other hand, the PMP crystal has a void width of approximately 4 Å as estimated by X-ray diffraction, so it was anticipated that CO2 would be able to sorb into the PMP crystal while C3H8 would not. The data show that C3H8 has a constant partial molar volume of approximately 87 cc/mol, just above the value reported in other rubbery polymers, and are consistent with the hypothesis that the C3H8 molecules are too large to sorb into the PMP crystals. The partial molar volume of CO2 was found to be 39 cc/mol for CO2 weight fractions of up to 0.03. Since the typical partial molar volume of CO2 in rubbery materials is 46 cc/mol, the lower values in this study were attributed to CO2 sorption into crystalline regions of the polymer, which provided no dilation. Application of a two-phase model using the assumption of Henry's law sorption showed that apparently all C3H8 sorption was occurring in the amorphous region but approximately 16% of CO2 sorption occurred in the crystalline regions. © 1996 John Wiley & Sons, Inc. 相似文献
13.
A. A. Bogolyubov N. B. Chernysheva V. V. Nesterov M. Yu. Antipin V. V. Semenov 《Chemistry of Heterocyclic Compounds》2004,40(10):1305-1309
The dehydration of two 5,5-disubstituted 4-hydroxy-4-methyl-3-phenylaminooxazolidin-2-ones into the corresponding 4-methylene-3-phenylaminooxazolidin-2-ones has been carried out. The structure of the products was confirmed by X-ray diffraction analysis.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1512–1517, October, 2004. 相似文献
14.
Alessandro D'Aprano Ines Dorina Donato Vincenzo Turco Liveri 《Journal of solution chemistry》1989,18(8):785-793
Static dielectric constants, refractive indices and viscosities of 1-pentanol +2-methyl-2-butanol mixtures were measured at 5, 25 and 45°C. The results show that the mixing of the two isomers modifies the polarizability and the resistence of viscous flow of the system depending on the composition and temperature. Short range intermolecular interactions producing hetero-alcohol open dimers are considered. 相似文献
15.
Yughandhar Sreedhar Neelam Rekha Dasari P. Reddy Prasad M. Sankar Nayak 《Journal of Saudi Chemical Society》2010,14(2):149-155
A novel analytical reagent 4-(2-hydroxy phenyl ethaminodiol), benzene-1,3-diol(4-2-HPEDB-1,3,D) was synthesized for the determination of molybdenum(VI). The present paper reveals the detailed study of electroanalytical behaviour for [Mo-(4-2-HPEDB-1,3,D)] complex under optimized conditions. The peak obtained for [Mo-(4-2-HPEDB-1,3,D)] prevent the interference of foreign ions which shows the sensitivity of the proposed method. The linearity was maintained at the concentration range of 0.5–200 μg/mL at pH 4.5 with correlation factor 0.9997. The present method was successfully applied for the analysis of molybdenum(VI) in biological fluids and plant material. The results obtained from the proposed method show good agreement with reference method. 相似文献
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17.
Titanium(IV) in sulphuric, perchloric and hydrochloric acid media reacts with 3-hydroxy-2-methyl-1-(4-tolyl)-4-pyridone (HY) to give a complex which is extractable into chloroform. The composition of the extractable complex depends on the acidity of the aqueous phase and on which mineral acid is used. The mixed titanium-perchlorate-HY complex which is formed in the presence of excess of perchlorate is the most suitable for the spectrophotometric determination of titanium. The molar absorptivity of the complex is 1.6×1041·mole–1·cm–1 at 355 nm. The optimum titanium concentration range is 0.5–6,g/ml. The method has been successfully applied to the determination of titanium in samples of bauxite and alumina refractory. 相似文献
18.
Vasil Andruch Monika Telepc˘áková Ioseph S. Balogh Nikoleta Urbanová 《Mikrochimica acta》2003,142(1-2):109-113
The complex formation and extraction of chromium(VI) with 2-[2-(4-methoxy-phenylamino)-vinyl]-1,3,3-trimethyl-3H-indolium
chloride reagent was studied by means of spectrophotometry. The influence of medium acidity, the concentration of chloride
ions and dye reagent, the nature of the extractant and some other factors (time of extraction, stability of color, interference,
etc.) on the absorbance of colored extracts were studied. The optimum conditions were found to be 0.02–0.1 M H2SO4, 1.0–1.5 M NaCl, (2.0–2.5) × 10−4 M of reagent. The absorbance of the colored extracts obeys Beer’s Law in the range of 0.26–7.28 mg L−1. The procedure of Cr(VI) extraction and spectrophotometric determination was examined.
Author for correspondence. E-mail: andruch@kosice.upjs.sk
Received November 19, 2002; accepted March 10, 2003
Published online June 13, 2003 相似文献
19.
Synthesis,Structure, Bonding,and Reactivity of Metal Complexes Comprising Diborane(4) and Diborene(2): [{Cp*Mo(CO)2}2{μ‐η2:η2‐B2H4}] and [{Cp*M(CO)2}2B2H2M(CO)4], M=Mo,W 下载免费PDF全文
Dr. Bijan Mondal Ranjit Bag Sagar Ghorai Dr. K. Bakthavachalam Prof. Eluvathingal D. Jemmis Prof. Sundargopal Ghosh 《Angewandte Chemie (International ed. in English)》2018,57(27):8079-8083
The reaction of [(Cp*Mo)2(μ‐Cl)2B2H6] ( 1 ) with CO at room temperature led to the formation of the highly fluxional species [{Cp*Mo(CO)2}2{μ‐η2:η2‐B2H4}] ( 2 ). Compound 2, to the best of our knowledge, is the first example of a bimetallic diborane(4) conforming to a singly bridged Cs structure. Theoretical studies show that 2 mimics the Cotton dimolybdenum–alkyne complex [{CpMo(CO)2}2C2H2]. In an attempt to replace two hydrogen atoms of diborane(4) in 2 with a 2e [W(CO)4] fragment, [{Cp*Mo(CO)2}2 B2H2W(CO)4] ( 3 ) was isolated upon treatment with [W(CO)5?thf]. Compound 3 shows the intriguing presence of [B2H2] with a short B?B length of 1.624(4) Å. We isolated the tungsten analogues of 3 , [{Cp*W(CO)2}2B2H2W(CO)4] ( 4 ) and [{Cp*W(CO)2}2B2H2Mo(CO)4] ( 5 ), which provided direct proof of the existence of the tungsten analogue of 2 . 相似文献
20.
Reaction between the title compounds gave the unexpected 3-[5,5-dimethyl-2,5-dihydrofur-4-yl-2-(3-isopropanol-2-propenonitrile)imino]benzothiazol-2-one, as a result of the addition of two cyanoacetylene molecules.Irkutsk Institute of Organic Chemistry, Siberian Branch, Russian Academy of Sciences, Irkutsk 664033. Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 4, pp. 1003–1005, April, 1992. 相似文献