- Method for continuously dropwise adding benzenyl trichloride to synthesize benzoyl chloride
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The invention provides a method for continuously dropwise adding benzenyl trichloride to synthesize benzoyl chloride, and relates to the technical field of fine chemical synthesis, the method comprises the following steps: (1) carrying out a chlorination reaction on toluene and chlorine to prepare a benzenyl trichloride crude product; (2) continuously dropwise adding the benzenyl trichloride crudeproduct obtained in the step (1) into benzoic acid for synthesis reaction to prepare a benzoyl chloride crude product; (3) carrying out reduced pressure rectification on the benzoyl chloride crude product prepared in the step (2), and collecting the fraction to obtain a benzoyl chloride fine product; raw materials are easy to obtain and low in price, operation is simple, energy consumption is low, content is high, quality is stable, production cost is low, three wastes are less, the total yield of the product is 94-96%, the purity is more than 99%, and the method is suitable for industrial production and has a good application prospect.
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Paragraph 0024; 0025; 0028; 0029; 0032; 0033
(2019/05/16)
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- Synthetic process for benzoyl chloride
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The invention relates to a synthetic process for benzoyl chloride, and belongs to the technical field of preparation of the benzoyl chloride. The synthetic process comprises the following steps: (1) adding a side reaction inhibitor under irradiation of an LED light source, introducing chlorine gas into toluene, and performing a reaction to obtain crude benzotrichloride, wherein the wavelength of the LED light source is 520-650 nm, and the side reaction inhibitor is a mixture of 4,6-dinitro-2-sec-butylphenol and aniline; (2) adding benzoic acid, adding the crude benzotrichloride obtained in thestep (1) dropwise under the action of a catalyst, and performing a reaction at 110-120 DEG C to obtain crude benzoyl chloride; and (3) performing reduced-pressure distillation purification on the crude benzoyl chloride obtained in the step (2) to obtain the refined benzoyl chloride. The synthetic process provided by the invention has the advantages of simple operation, a short reaction period, alow reaction temperature, low energy consumption, a high product yield, high product purity and low production costs, and is suitable for industrialized production.
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Paragraph 0029-0030; 0032-0033; 0035-0036; 0038-0039
(2019/07/16)
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- CLEAN PROCESS FOR PREPARING CHLOROFORMYL-SUBSTITUTED BENZENE
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Clean process for preparing a chloroformyl-substituted benzene by oxidation of a tail gas hydrogen chloride from a chlorination reaction and a chloroacylation reaction and recycling of the resulting oxidation product chlorine gas into the chlorination reaction. The present invention provides a clean process for preparing a polymer-grade chloroformyl-substituted benzene.
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Paragraph 0125; 0139; 0151; 0163
(2017/12/17)
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- Catalytic halodefluorination of aliphatic carbon-fluorine bonds
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A variety of halosilanes, in conjunction with aluminum catalysts, convert fluorocarbons into higher halocarbons. Bromination and iodination of fluorocarbons are more effective than chlorination in terms of yield and activity. The mechanism for the reaction is investigated utilizing experimental and computational evidence and preliminary results suggest an alternate mechanism to that reported for the related hydrodefluorination reaction.
- Goh, Kelvin K.K.,Sinha, Arup,Fraser, Craig,Young, Rowan D.
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p. 42708 - 42712
(2016/05/19)
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- METHOD FOR THE PREPARATION OF TRICHLOROMETHYL-GROUP-SUBSTITUTED BENZENE
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The present application relates to a method for photochlorination, and specifically to photochlorination by a photochemical reaction of an aromatic compound with gaseous chlorine so as to prepare a trichloromethyl-substituted benzene, and to a method using bis-(trichloromethyl)-benzene as the trichloromethyl-substituted benzene to prepare by further reaction bis-(chloroformyl)-benzene. Through the control of temperature, illuminance and consumption of gaseous chlorine, the method of this application can greatly improve the purity of trichloromethyl-substituted benzene and further prepare polymer-grade bis-(chloroformyl)-benzene with low cost. The present application also relates to a method for purifying trichloromethyl-substituted benzene, and specifically to a method for purifying trichloromethyl-substituted benzene via molecular distillation. The present application further relates to a photochlorination reactor for use in photochlorination reactions (such as those of the present application).
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Paragraph 0157
(2016/06/28)
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- Process for the preparation of benzoyl chloride
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The invention relates to a preparation method of benzoyl chloride and belongs to the technical field of the preparation of the benzoyl chloride. The preparation method of the benzoyl chloride comprises the following steps: (1) under the irradiation of an LED light source, firstly, adding a side reaction inhibitor, and then introducing chlorine into methylbenzene, and performing a heating and stirring reaction to obtain the crude product of benzyl trichloride; (2) heating benzoic acid for melting, and in the presence of a catalyst, adding the crude product of the benzyl trichloride obtained in the step (1) for reacting to obtain the crude product of benzoyl chloride; (3) purifying the obtained crude product of the benzoyl chloride by virtue of reduced pressure distillation, thereby obtaining the refined benzoyl chloride. The preparation method of the benzoyl chloride is simple to operate, short in reaction period, low in energy consumption, high in product purity and yield, low in production cost and suitable for industrial production.
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Paragraph 0046
(2017/03/08)
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- Method of manufacturing hydroxybenzenesulfonic deriv. Halomethylation
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PROBLEM TO BE SOLVED: To provide a method for producing a halomethylbenzene derivative by halogenating a methylbenzene derivative at the benzyl position, which is industrially achievable. SOLUTION: In the method for producing a halomethylbenzene derivative represented by formula (2) (wherein R1-R5are each independently a hydrogen atom, tert-butyl, phenyl or the like; X, Y and Z are each independently a halogen atom; p and q are each independently 0, 1 or 2; z is 1, 2 or 3 and p+q+z is 1, 2 or 3) by halogenating a methylbenzene derivative by light or heat, halogenation is carried out in a chain fluorine-containing hydrocarbon or cyclic fluorine-containing hydrocarbon. COPYRIGHT: (C)2011,JPOandINPIT
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Paragraph 0034; 0043
(2016/10/20)
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- Non-catalytic conversion of C-F bonds of benzotrifluorides to C-C bonds using organoaluminium reagents
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A facile method for the conversion of C-F bonds of benzotrifluorides to C-C bonds has been developed using aluminium reagents in the absence of catalysts.
- Terao, Jun,Nakamura, Misaki,Kambe, Nobuaki
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supporting information; experimental part
p. 6011 - 6013
(2010/11/16)
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- Inter- and innermolecular reactions of chloro(phenyl)carbene
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Supramolecular photolyses of 3-chloro-3-phenyl-3H-diazirine (8) were performed within cyclodextrin (CyD) hosts to determine whether these toroidal inclusion compounds could alter the reactivity of the ensuing carbene reaction intermediate, chloro(phenyl)carbene (9). Remarkably, no intramolecular products stemming from carbene 9 could be detected. Instead, modified CyDs were formed via so-called innermolecular reactions. Hence, diazirine 8 was photolyzed in various conventional solvents to gauge the intermolecular reactivity of carbene 9. Relevant results were used to rationalize the CyD innermolecular reaction products.
- Rosenberg, Murray G.,Brinker, Udo H.
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p. 4819 - 4832
(2007/10/03)
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- Stabilities of complexes of Br- with substituted benzenes (SB) based on determinations of the gas-phase equilibria Br- + SB = (BrSB)-
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Equilibria involving some forty substituted benzenes (SB) and the bromide ion (SB + Br- = SBBr-) in the gas phase were determined with a pulsed electron, high-pressure mass spectrometer (PHPMS). The resulting -ΔG°1 provide information on the stabilities of the SBBr- complexes. Previous work, involving gas-phase thermochemical data for. X- (CH3O-, F-, C1-, Br-, I-) and quantum chemical calculations, indicate that the most stable SB·X- complexes might have a variety of structures, depending on X- and the nature of the substituents. Thus X- may engage in hydrogen bonding to an aromatic hydrogen atom, or lead to a σ-bonded (Meisenheimer) complex, or form a complex where X- is on an axis perpendicular to the benzene plane. A Taft substituent analysis of the δΔG°1 indicates that Br- and Cl- form aromatic C-H hydrogen-bonded complexes with all singly substituted benzenes. The field effects of the substituents provide the dominant contribution to the bonding in these complexes. Similar conclusions are reached also for the singly substituted nitrobenzenes and Br-. A clearcut analysis of the bonding to Br- when triply substituted benzenes with strongly electron withdrawing substituents like CF3, CN, and NO2 are present could not be obtained. In these cases all three bonding structures mentioned above may have similar stabilities.
- Paul, Gary J. C.,Kebarle, Paul
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p. 1148 - 1154
(2007/10/02)
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- Preparation of substituted benzotrichlorides
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A process for chlorinating a compound of the formula STR1 in which R1 is a C1 -alkyl radical, C1 -alkoxy radical or C1 -thioalkyl radical, and X1, X2, X3 and X4 are identical or different hydrogen or halogen, and X3 may alternatively be STR2 or --NCO, comprising, in an initial phase, dissolving a chlorination catalyst in the compound to be chlorinated, continuously metering this solution together with chlorine into a reaction vessel containing the compound to be chlorinated, and, after the initial phase, removing partially or fully chlorinated compounds from the reaction vessel, dissolving fresh chlorination catalyst in the removed compounds, and feeding this catalyst solution, together with chlorine, to the reaction vessel.
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- Versatility of Zeolites as Catalysts for Ring or Side-Chain Aromatic Chlorinations by Sulfuryl Chloride
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Zeolites catalyze chlorination of aromatics by sulfuryl chloride SO2Cl2.It is possible by an appropriate choice of the catalyst to effect at will, with very high selectivity, either the ring or the side-chain chlorination.Zeolite ZF520 is the choice catalyst for the former, because of its high Broensted acidity.Zeolite NaX (13X) is a fine catalyst for the latter, free-radical chlorination; the reaction is best effected in the presence of a light source; the catalyst can be reused many times with no loss in activity.Both reaction modes, the ionic (ring chlorination)and the radical (side-chain substitution), are likely to occur outside of the channel network in the microporous solid.The effects of various experimental factors - such as the nature of the solvent, the reaction time and temperature, the Broensted acidity of the solid support, the presence of radical inhibitors, and the quantity of catalysts - were investigated.The procedures resulting from this study are very easy to implement in practice and are quite effective.
- Delaude, Lionel,Laszlo, Pierre
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p. 5260 - 5269
(2007/10/02)
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- Processes using a phosphorus complex
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A process for chlorinating compounds containing a carbon atom bonded to a hetero-atom selected from the group consisting of oxygen, nitrogen and sulfur; said process comprises contacting the carbon hetero-atom containing compound with a chloro phosphorus complex of the formula wherein R is selected from the group consisting of aryl, substituted aryl, alkyl and substituted alkyl, so that the hetero-atom is replaced by at least one chlorine atom; compounds capable of being chlorinated can include, for example, carboxylic acids, acid chlorides, ketones, aldehydes, alcohols, epoxides, esters, anhydrides, ethers, thiols, and aromatic nitro groups; the reaction can be extended to compounds containing the carbon to chlorine bond alpha to a carbon atom containing at least one hydrogen atom, it can be further dehydrochlorinated, e.g., by either heating to a temperature ranging from about 50° C. to about 300° C. or by reaction with a base selected, e.g., from alkali metal hydroxides and alkoxides.
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- THE PHASE TRANSFER CATALYSED PREPARATION OF 2-METHYL-2-TRICHLOROMETHYL-3-PHENYLOXIRANE
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A phase transfer catalyst has been used to prepare the title compound and other highly chlorinated compounds from phenylpropanone and carbon tetrachloride.
- Reeves, W. Preston,Creswell, Mark W.
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p. 945 - 950
(2007/10/02)
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- SPONTANEOUS RADICAL CHLORINATION OF TOLUENE IN THE SIDE CHAIN
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The effect of oxygen on the rate of radical chlorination of toluene in the side chain was investigated.It was shown that if oxygen dissolved in the toluene is removed by blowing the toluene with inert gass (carbon dioxide or nitrogen) and chlorine not con
- Serguchev, Yu. A.,Moshkin, V. F.,Konoval, Ya. V.,Stetsyuk, G. A.
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p. 908 - 910
(2007/10/02)
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- SELECTIVITY OF FREE-RADICAL CHLORINATION OF BENZYL CHLORIDE AND BENZYLIDENE CHLORIDE
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The competition between substitutive and additive chlorination of benzyl and benzylidene chlorides was investigated.It was shown that the proportion of substitutive chlorination increases with decrease in the concentration of chlorine and with increase in temperature.A mechanism is proposed which involves the formation of ? complexes of the chlorine atoms with the aromatic substrates followed by rearrangement to ? complexes.An equation for the selectivity of the investigated processes was obtained on the basis of the proposed mechanism.
- Aver'yanov, V. A.,Kirichenko, S. E.,Shvets, V. F.
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p. 1840 - 1844
(2007/10/02)
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