- Synthesis and crystal structure of 3,5-dichloro-6-morpholinopyridin-2-ol
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A new compound having potential bioactivities 3,5-dichloro-6- morpholinopyridin-2-ol (1) was synthesized and characterized by single crystal X-diffraction. The crystal is monoclinic, space group P21/c with a = 10.3609 (6), b = 10.5711 (7), c = 10.3190 (5) A, β = 108.9433 (15)°, V = 1068.99 (11) A3, Z = 4, C9H 10Cl2N2O2, D c = 1.548 g/cm3, μ (MoKα) = 0.71075 A, S = 1.01, F (000) = 512.00, R = 0.0397 and wR = 0.1364. In the unit cell, there are two independent molecules linked by intermolecular O-H???O (2.693(2) A) hydrogen bonds forming onedimensional expanded structure. Graphical Abstract: As part of our ongoing research work on pyridine derivatives, the title compound crystal structure is important to study the relationship between the structure and its biological activities, thus it is urgent to publish in time.[Figure not available: see fulltext.]
- Zheng, Hui,Liu, Yun-Kui,Shen, Chao,Xu, Zhen-Yuan
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- Effect of nitrogen-containing compounds on polychlorinated dibenzo-p-dioxin/dibenzofuran formation through de novo synthesis
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An experimental study was conducted to clarify the suppression effect of nitrogen-containing compounds, that is, ammonia and urea, on the formation of polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) through the de novo synthesis reaction. In the experiment, graphite and copper chloride contained in a mixture were used as sources of carbon and chlorine, respectively. The granulated sample mixture was charged as a packed-bed in the glass tube and heated at 300 °C in the flow of Ar-O 2 gas mixture. In some cases, urea was added as aqueous solution to the sample, while ammonia was added to the gas flowed through the sample bed. The amount of PCDD/Fs formed decreases significantly by the addition of both ammonia and urea. Particularly, the addition of urea reduces the amount of PCDD/Fs discharged in the outlet gas by approximately 90%. The oxidation rate of carbon in the early stage of the experiment, that is, the heating period, is promoted by the addition of nitrogen-containing compounds. However, soon after the temperature reaches 300 °C, the formation rate becomes lower than that of the case without the addition of nitrogen-containing compounds. On the other hand, organic compounds containing amino (-NH2) or cyanide (-CN) groups and those containing nitrogen within the carbon ring frame were detected in the outlet gas in the case of urea addition. Typically observed aromatic compounds are chlorobenzonitriles, chlorobenzeneamines, and chloropyridines. This suggests a possibility that hydrogen and/or chlorine combined with PCDD/Fs are also substituted by such nitrogen-containing groups, and this decreases the formation rate of their frame of carbon rings. This phenomenon was also consistent with the fact that a significant reduction was observed in the amount of PCDD/Fs released to the outlet gas when urea was added.
- Kuzuhara, Shunsuke,Sato, Hiroshi,Tsubouchi, Naoto,Ohtsuka, Yasuo,Kasai, Eiki
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p. 795 - 799
(2007/10/03)
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- Mild electrophilic halogenation of chloropyridines using CCl4 or C2Cl6 under basic phase transfer conditions
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Effective chlorination of 2,3,5,6-tetrachloropyridine to pentachloropyridine was realized under mild phase transfer conditions with carbon tetrachloride and 50% NaOH or solid K3PO4. Mechanistic study of this reaction indicated the possibility of an aromatic carbanionic intermediate. Hexachloroethane was established as a more selective electrophilic chlorination agent.
- Joshi, Ashutosh V.,Baidossi, Mubeen,Qafisheh, Nida,Chachashvili, Elsa,Sasson, Yoel
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p. 5061 - 5063
(2007/10/03)
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- Organochlorine formation in magnesium electrowinning cells
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The formation of organochlorines during the electrolytic production of magnesium was investigated using a laboratory-scale electrolytic cell having a graphite anode, a liquid aluminium alloy cathode, and a molten chloride electrolyte. The cell was operated at current densities ranging from 3000 to 10,000 A m-2 and at temperatures ranging from 660°C to 750°C. Organochlorines were adsorbed from the cell off-gases onto silica gel, extracted with hexane, and determined by gas chromatography. All compounds identified were fully chlorinated aliphatic and aromatic compounds, the major components being hexachlorobutadiene, hexachlorobenzene, hexachloroethylene, and octachlorostyrene. The total amount of organochlorines per tonne of magnesium produced decreased with electrolysis time and with current density and increased with operating temperature; it was also dependent on the type of graphite employed. The output of organochlorines Varied from 5 to 20 g t-1 of magnesium.
- Deutscher,Cathro
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p. 147 - 155
(2007/10/03)
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- Thermolysis of phenoxyaluminum compounds and formation of PCDD/F and their precursors
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Within the study of the formation of chlorinated dioxins and dibenzofurans and their precursors the thermolysis of hexachloroethane over the aluminum melt was investigated. "De novo" synthesis of precursors of PCDD/F was studied in the model system AlCl3/elemental carbon. Totally chlorinated heterocyclic compounds have been detected parallel with the formation of organochlorine compounds. The possibility of inserting oxygen to aluminum organyls was presented. In order to gain more detailed knowledge of the catalytic behaviour of fly ash the chemistry of thermolysis of phenoxy- and chlorophenoxy aluminum compounds at 300°C with the presence and absence of Al2O3 was investigated. Reagent compounds and products of thermolysis were followed by mass spectrometry.
- Voncina,Medved,Zerjal
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p. 2029 - 2038
(2007/10/03)
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- DESTRUCTIVE CHLORINATION OF 3,4,5-TRICHLORO-2-(TRICHLOROMETHYL)PYRIDINE
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The extensive destructive chlorination of 3,4,5-trichloro-2-(trichloromethyl)pyridine proceeds by both thermal (160-245 deg C) and photochemical pathways.Perchloropyridine, perchloropicoline, and carbon tetrachloride are formed.The chlorinated derivatives of pyridine are formed by the loss of the CCl3 group with its subsequent replacement by a chlorine atom.
- Emel'yanov, V. I.,Stul', B. Ya.,Korolev, B. M.
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p. 1168 - 1171
(2007/10/02)
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- Polyhalogenoaromatic Compounds. Part 41. Photochemical Dehalogenation and Arylation Reactions of Polyhalogenoaromatic and Polyhalogenoheteroaromatic Compounds
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Photolysis of pentachloro- and pentabromo-pyridine in diethyl ether or methanol leads to loss of β-halogen.A product (9) derived from attack on diethyl ether was also identified. 4-Bromotetrachloropyridine also undergoes loss of bromine and tetrachloro-4-iodopyridine loses iodine exclusively.Photodehalogenation of some perhalogenothiophens, tetrachloropyrimidine, and hexachlorobenzene is also described.Photolysis of pentachloroiodobenzene, tetrachloroiodopyridines, and trichloro-5-iodothiophen in benzene gives the corresponding polychloroaryl- or polychloroheteroaryl-benzenes.Photolysis of tetrachloro-4-(phenylthio)pyridine (3) gives 1,3,4-trichlorobenzothienopyridine (6), and the analogous perchloro(phenylthio)pyridine (37) gives the corresponding perchlorobenzothienopyridine (61).The scope of this type of photocyclisation has been explored; starting materials investigated include various arylthiopolyhalogenopyridines, some arylamino- and aryloxy-tetrachloropyridines, and 4-anilinotrichloropyrimidine.
- Bratt, Jack,Iddon, Brian,Mack, Arthur G.,Suschitzky, Hans,Taylor, Jack A.,Wakefield, Basil J.
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p. 648 - 656
(2007/10/02)
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- Polyhalogenoaromatic Compounds. Part 43. Inter- and Intra-molecular Reactions of Polychloroaromatic Compounds with Copper
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The reaction of polychloroiodoarenes with copper in dimethylformamide gives good yields of the biaryls. 4-Bromotetrachloropyridine gives products of halogen exchange and reduction as well as coupling.Pentachloropyridine gave only tetrachloropyridines.Evidence against free radical or pyridyne intermediates is presented, and it is postulated that the reactions proceed via pyridylcopper compounds, although an electron transfer mechanism is not excluded.On reaction with copper, some 4-(o-halogenophenoxy)- and 4-(o-halogenothiophenoxy)-tetrahalogenopyridines give products of cyclisation, reduction, and halogen transfer.Copper reacts initially, at least in part, with the pyridyl group rather than with the o-halogenoaryl group.The results are again consistent with a reaction pathway involving a pyridylcopper intermediate.The products of nucleophilic substitution in pentahalogenopyridines by some phenols, thiophenols, and anilines are reported.
- Mack, Arthur G.,Suschitzky, Hans,Wakefield, Basil J.
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p. 1682 - 1687
(2007/10/02)
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- Polyhalogenoaromatic Compounds. Part 44. Reactions of Enamines with Polyhalogenopyridines and their N-Oxides
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1-Dialkylaminocyclohexenes were readily C-arylated by pentafluoropyridine or 3,5-dichlorotrifluoropyridine but pentachloropyridine was much less reactive.The resulting (tetrahalogenopyridyl)enamines did not cyclise on heating except in the case of compound (10), which gave the heterocycle (16). 1-Dialkylaminocycloalkenes and other enamines were C-arylated by pentachloropyridine N-oxide.In the cases of the dialkylaminocyclo-hexenes and -heptenes the expected pyridylenamines were accompanied by 1-(tetrachloro-2-pyridyl)cyclo-pentene and -hexene, respectively.A mechanism for the ring-contraction leading to the pyridylcycloalkenes is proposed involving a novel elimination of an N-formyldialkylamine.
- Suschitzky, Hans,Wakefield, Basil J.,Whitten, Jeffrey P.
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p. 2709 - 2716
(2007/10/02)
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