- METHOD FOR PREPARING 2-METHYLALLYL CHLORIDE FROM 1,2-DICHLOROTERT-BUTANE
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The present invention relates to a method for preparing 2-methylallyl chloride from 1,2-dichloro-tert-butane. The method is characterized in that 1,2-dichloro-tert-butane and a sodium hydroxide aqueous solution are used as raw materials; reactive rectification is performed in a combined rectifying tower to eliminate hydrogen chloride so as to obtain 2-methylallyl chloride. A plate type tower is provided at the lower part of the combined rectifying tower; a packing tower is provided at the upper part of the combined rectifying tower; an inner reflux condenser is provided at the top of the combined rectifying tower. The sodium hydroxide aqueous solution is added from a first plate of the plate type tower; and 1,2-dichloro-tert-butane is added from the middle part of the plate type tower. The method has the advantages that the raw material 1 and 1,2-dichloro-tert-butane is fully converted; the selectivity of the 2-methylallyl chloride is high.
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Paragraph 0026
(2021/11/26)
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- Method for co-producing methyl chloropropene and 2-chloro-2-methylpropane by chlorination of isobutene
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The invention discloses a method for co-producing methyl chloropropene and 2-chloro-2-methylpropane by chlorination of isobutene. According to the method, a chlorination reaction is carried out on chlorine or a mixture of chlorine and inert gas and excessive isobutene to obtain products, namely methyl chloropropene and 2-chloro-2-methylpropane. The method can reduce influence of micro-mixing on arapid chlorination reaction of isobutene, decarburization and coking do not occur easily, and 2-chloro-2-methylpropane can be co-produced while the yield of methyl chloropropene is improved.
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Paragraph 0025; 0026
(2020/01/12)
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- Chlorinating preparation method for low-carbon olefins
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The invention discloses a chlorinating preparation method for low-carbon olefins. According to the method, chlorine gas is diluted with inert gas and then reacts with low-carbon olefins, thus, influence caused by microscopic mixing can be obviously reduced, namely, a too high local temperature can be avoided, thus, side reactions including a decarbonization phenomenon caused by the too high localtemperature can be obviously reduced, and a relatively good chloride yield can be obtained.
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Paragraph 0037-0039
(2020/01/12)
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- Process for functionalising a phenolic compound carrying an electron-donating group
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The invention concerns a method for functionalizing a phenolic compound bearing an electron-donor group, in said group para position, inter alia a method for the amidoalkylation of a phenolic compound bearing an electron-donor group, and more particularly, a phenolic compound bearing an electron-donor group preferably, in the hydroxyl group ortho position. The method for functionalizing in para position with respect to an electron-donor group carried by a phenolic compound is characterised in that the phenolic compound bearing an electron-donor group is subjected to the following steps: a first step which consists of protecting the hydroxyl group in the form of a sulphonic ester function; a second step which consists in reacting the protected phenolic compound with an electrophilic reagent; optionally, a third step deprotecting the hydroxyl group.
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- Esterification of carboxylic acid salts
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Mono- or polycarboxylic acid esters are prepared by reacting a salt of such carboxylic acid with an organic halocompound, e.g., a (cyclo)alkyl, (cyclo)alkenyl, aryl or aralkyl halide, in an aqueous reaction medium, in the presence of a catalytically effective amount of a phase transfer catalyst, for example an onium salt.
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- Quaternary ammonium polychlorides as efficient reagents for chlorination of unsaturated compounds
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Chlorination of unsaturated compounds by benzyltributylammonium polychlorides results in higher yields of addition products compared to those obtained with molecular chlorine.
- Zelikman,Tyurin,Smirnov,Zyk
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p. 1541 - 1546
(2007/10/03)
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- 1,1-dicyclohexyl cycloalkane derivative, method for the preparation thereof and traction-drive fluid containing the same
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The invention provides a novel compound 1,1-dicyclohexyl cycloalkane derivative represented by the general formula STR1 in which R1 and R2 are each a hydrogen atom or lower alkyl group, R3 to R6 are each a hydrogen atom, lower alkyl group or alkylene group forming a ring structure together with either one of the others and the carbon atom in the cycloalkane ring, and m and n are each zero or a positive integer not exceeding 6 with the proviso that m+n is 4-6, such as 1,1-dicyclohexyl cyclohexane. The compound has a relatively low viscosity and high traction coefficient even at elevated temperatures so that it is useful as a constituent of a traction-drive fluid usable in a compact and light-weight traction-drive apparatus. The compound can be synthesized by subjecting a corresponding 1,1-di(hydroxyphenyl) cycloalkane compound to a hydrogenation reaction and dehydration reaction in combination in the simultaneous presence of a hydrogenation catalyst and a dehydration catalyst.
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- Process for manufacturing methallyl chloride
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A method for manufacturing methallyl chloride by reacting isobutene with chlorine in the gas phase is disclosed. The reaction is carried out in a distributed nozzle-mixing reactor which enables the reaction to proceed in a stabile manner even without addition of oxygen. At the same time, the yield of methallyl chloride is increased.
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- Reductive elimination of η3-allyl(aryl)palladium complexes promoted by allyl halides
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Comparison between the reactivity patterns of the reactions of μ3-allyl(aryl)palladium complexes with allyl chlorides and those with styrene, allylbenzene, methyl iodide and benzyl chloride suggested the dual role of allyl chloride in enhancing the reductive elimination of these complexes, namely coordination to Pd through the C=C bond and removal of the electron density via oxidative addition.The product distribution pattern in the reductive elimination of Pd(η3-CH2CHCH2)(Ar)(EPh3) (1) (E=P, As; Ar=C6H3Cl2-2,5) accelerated by CH2=CMeCH2Cl (reaction A) and that of Pd(η3-CH2CMeCH2)(Ar)(EPh3) (2) accelerated by CH2=CHCH2Cl (reaction B) has been determined.For the reaction of the AsPh3 complexes, both A and B carried out in toluene and dichloromethane afforded, at the early stages, only the coupling product (allylbenzene derivative) associated with the allyl unit of the original complex itself.At the later stages the product derived from the substrate chloride increased owing to facile ligand exchange (allyl-methallyl and/or aryl-Cl) between 1 and 2 and the η3-allyl(chloro)palladium complex which is another product of the reductive elimination.Consistent with the oxidative addition of the allyl chlorides, the reaction of the PPh3 complexes in dichloromethane and 1,2-dichloroethane gave a greater quantity of the product derived from the substrate chloride than that from the complex even at the early stages.
- Kurosawa, Hideo,Emoto, Mitsuhiro,Kawasaki, Yoshikane
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p. 137 - 146
(2007/10/02)
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- Influence of Polar α Substituents in the Gas-Phase Pyrolysis Kinetics of Tertiary Chlorides. Correlation of Alkyl and Polar Groups
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The kinetics of the gas-phase pyrolysis of several polar α-substituted tertiary chlorides were determined in a static system over the temperature range of 339.5-420.1 deg C and the pressure range of 46-221 torr.The reactions in seasoned vessels and in the presence of a free-radical suppressor, are homogeneous and unimolecular and follow a first-order rate low.The variation of the rate coefficients with temperature is given by the following Arrhenius equations: for 1,2-dichloro-2-methylpropane, log k1 (s-1) = (14.29 +/- 0.53) - (207.6 +/- 6.4) kJ mol-1 (2.303RT)-1; for 2,2-dichloropropane, log k1 (s-1) = (12.88 +/- 0.53) - (199.0 +/- 6.5) kJ mol-1 (2.303RT)-1; for methyl 2-chloro-2-methylpropionate, log k1 (s-1) = (13.81 +/- 0.26) - (215.2 +/- 3.3) kJ mol-1 (2.303RT)-1.The log krel of polar α substituents against the polar substituent constant ?* values give an approximate straight line with ρ* = -0.73, correlation coefficient r = 0.912, and intercept = -0.194 at 300 deg C.This slope inflects at the point where ?*(CH3) = 0.00 with another reported very good straight line derived by plotting log k/k0 vs. ?* values for 2-chloro-2-alkylpropane pyrolyses (ρ* = -4.75, r = 0.993, and intercept = 0.047 at 300 deg C).The present results has been rationalized, as before, in terms of a slight alteration in the polarity of the transition state due to changes in electronic transmission at the carbon reaction center.
- Chucani, Gabriel,Rotinov, Alexandra,Martin, Ignacio,Avila, Irama,Dominguez, Rosa M.
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p. 4134 - 4137
(2007/10/02)
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- Decarboxylase-inhibiting fluorinated pentane diamine derivatives
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Novel fluorinated diamine derivatives are inhibitors of ornithine decarboxylase enzyme and have the following general Formula I: STR1 wherein: Rc represents hydrogen or carboxy; R1 represents hydrogen or C1 -C6 alkyl; Z represents methylene or oxygen; m and n each represent 0 or 1 but m+n=1; and p represents 1 or 2.
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- Synthesis and Characterization of Polychlorinated Isobutenes
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The preparation of polychlorinated methallylic chlorides by continuous chlorination of isobutene with different ratios of chlorine and following HCl-elimination is described.The structure is proved by reaction of the polychlorinated isobutenes with sodium thiolacetate and potassium thiocyanate and by spectroscopic methods.
- Schulze, K.,Hartmann, S.,Krueger, H.,Muehlstaedt, M.,Richter, C.,Richter, H.
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p. 433 - 442
(2007/10/02)
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- REACTION OF CYCLOPROPENE COMPOUNDS WITH BENZENESULFENYL CHLORIDES AND HYDROGEN CHLORIDE
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The reactions of 3,3-dimethylcyclopropene and 1-methylcyclopropene with 2,4-dinitrobenzene- and benzenesulfenyl chlorides and hydrogen chloride in acetic acid were investigated.It was shown that the reaction with benzenesulfenyl chlorides leads mainly to cyclic adducts, which are formed as a result of anti-addition of the reagent.Under the conditions of doping addition the predominant reaction path is the formation of the acyclic products.The addition of hydrogen chloride to the investigated hydrocarbons takes place entirely with ring opening.
- Kartashov, V. R.,Skorobogatova, E. V.,Akimkina, N. F.,Zefirov, N. S.
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- Synthesis and Properties of Some Metal β-Methalloxides
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Metal derivatives of β-methallyl alcohol having the general formulae M3, (M = B and Al); M4, (M = Ge and Ti); M5, (M = Nb and Ta) and BunSn4-n, (n = 1, 2 and 3) have been synthesized by alcohol interchange technique.Germanium tetra-β-methalloxide has been synthesized by the reaction of germanium tetrachloride with β-methallyl alcohol in the presence of dry ammonia as hydrogen chloride acceptor.These newly synthesized β-methalloxides are colourless liquids which can be distilled under reduced pressure.These derivatives have been characterized by elemental analyses, molecular weight determinations and IR as well as PMR spectral data.
- Goel, S. C.,Mehrotra, R. C.
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p. 440 - 442
(2007/10/02)
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- Novel indolobenzazepine derivatives, useful as tranquilizers
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Certain novel 1,2,3,4,8,9-hexahydro-3-(substituted)pyrido[4',3':2,3]indolo[1,7-ab][1]-benzazepines are useful as minor tranquilizers (anxiolytics) and/or major tranquilizers (antipsychotics). The minor tranquilizers are effective at non-ataxic doses, and are not likely to cause addiction when abused. A representative compound in this class is 3-(cyclopropylmethyl)-1,2,3,4,8,9-hexahydropyrido[4',3':2,3]indolo[1,7-ab][1]benzazepine.
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