76-02-8Relevant articles and documents
Direct Carbonylation of Polychloroalkanes into Acid Chlorides Using Metallic Salts Ternary Systems: an Example of Multistep Catalysis
Monflier, Eric,Mortreux, Andre,Petit, Francis,Lecolier, Serge
, p. 439 - 441 (1992)
A catalytic cycle for the direct carbonylation of CCl4 into CCl3COCl, catalysed by metallic salts mixtures. e.g.AlCl3/MCln/CuCl, under unexpectedly mild conditions, is proposed on the basis of FTIR, 17O and 27Al NMR spectroscopic studies.
Synthesis and Fungitoxic Evaluation of Acylamino-1,2,4-Triazoles
Kaur, Gurinderjit,Kaur, Harleen,Kaur, Pardeep,Sharma, Sunita,Singh, Ravneet
, p. 389 - 395 (2021/11/22)
Ten different acylamino-1,2,4-triazoles were prepared by the reaction of differently substituted benzoyl chlorides and acetyl chlorides with 4-amino-1,2,4-triazole using catalytic amount of triethylamine. The synthesized compounds were characterized using UV, 1H-nuclear magnetic resonance spectroscopy, and infrared spectroscopy. All the compounds were tested for their fungicidal potential against three fungal species, that is, Fusarium verticillioides, Macrophomina phaseolina, and Rhizoctonia solani using poisoned food technique. The synthesized compounds were tested at various concentrations along with standard carbendazim 50 WP. The amides synthesized by reaction of substituted benzoyl chlorides and 4-amino-1,2,4-triazole exhibited greater fungicidal activity against all the tested fungi as compared to the amides synthesized using substituted acetyl chlorides. Among all the tested compounds, 4-nitro-N-(4-H-1,2,4-triazol-4-yl)benzamide showed the maximum fungicidal activity with the least median effective dose (ED50) values of 100, 93, and 146 μg ml-1 against F verticillioides, M. phaseolina, and R. solani, respectively. All the compounds were found to be less effective than the standard used.
Synthesis method of chloroacetyl chloride
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Paragraph 0023; 0025, (2019/03/28)
The invention discloses a synthesis method of chloroacetyl chloride (ClCH2COCl). To be specific, the synthesis method is characterized in that an activated carbon loaded lewis acid catalyst is used for catalyzing gaseous acetyl chloride and chlorine to perform an alpha-halogenation reaction in a contact reactor to generate the chloroacetyl chloride. Lewis acid is specifically ferric chloride or aluminium chloride, and the consumption of the lewis acid is 1-7% of the total material input of acetyl chloride. The synthesis method disclosed by the invention is high in catalyst utilizing rate, highin selectivity, and less in byproducts, and the purity of a product is higher than or equal to 99.5%; the reaction is performed at low temperature; the energy consumption is low; the environmental pollution is small; and the reaction equipment structure is simple, and the operation is easy.
A high-purity 3, 5, 6 - trichloro-pyridine -2 - sodium alcoholate production process (by machine translation)
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Paragraph 0046; 0064, (2019/04/04)
The present invention relates to the technical field of chemical material production, and in particular relates to a high-purity 3, 5, 6 - trichloro-pyridine - 2 - sodium alcoholate production process, comprises the following steps: chlorine acetyl chloride; preparing trichlor; addition cyclization: the protection of inert gas atmosphere by adding solvent, the pure product of the chloroacetyl chloride, acrylonitrile and catalyst, the temperature of the stirred to back flow, so that the reflux to return to below the liquid level, reduced pressure distillation, heat filter, the catalyst can be recycled for use, get filtrate for use; preparing 3, 5, 6 - trichloro-pyridine - 2 - sodium alcoholate crude; for preparing high-purity 3, 5, 6 - trichloro-pyridine - 2 - sodium alcoholate. The invention solves the problems in the prior art 3, 5, 6 - trichloro-pyridine - 2 - sodium alcoholate preparation technical difficulty is high, the yield is low and low purity of, the prepared 3, 5, 6 - trichloro-pyridine - 2 - sodium alcoholate has high purity, high yield and relatively shallow the advantages of luster, reasonable production process and is favorable for industrial production. (by machine translation)
A synthetic method of trichloroacetyl chloride
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Paragraph 0033-0060, (2017/02/24)
A synthetic method of trichloroacetyl chloride is provided and belongs to the field of organic synthesis. The method includes steps of subjecting chlorine and chloroacetic acid in a melt state to a contact reaction to prepare a primary chlorination material, heating and reacting the primary chlorination material with sulfur monochloride and chlorine to prepare a secondary chlorination material, and heating and reacting the secondary chlorination material with chlorine under actions of a catalyst to obtain the trichloroacetyl chloride. The method synthesizes the trichloroacetyl chloride in a non-water system by utilizing the chloroacetic acid. The non-water system is adopted, thus avoiding generation of toxic and harmful compounds in a preparation process, avoiding a dewatering step, improving environment protection performance of the preparation process, simplifying the synthetic process and facilitating reduction of a synthesis cost.
A mild method for the replacement of a hydroxyl group by halogen. 1. Scope and chemoselectivity
Munyemana, Fran?ois,George, Isabelle,Devos, Alain,Colens, Alain,Badarau, Eduard,Frisque-Hesbain, Anne-Marie,Loudet, Aurore,Differding, Edmond,Damien, Jean-Marie,Rémion, Jeanine,Van Uytbergen, Jacqueline,Ghosez, Léon
, p. 420 - 430 (2015/12/31)
α-Chloro-, bromo- and iodoenamines, which are readily prepared from the corresponding isobutyramides have been found to be excellent reagents for the transformation of a wide variety of alcohols or carboxylic acids into the corresponding halides. Yields are high and conditions are very mild thus allowing for the presence of sensitive functional groups. The reagents can be easily tuned allowing therefore the selective monohalogenation of polyhydroxylated molecules. The scope and chemoselectivity of the reactions have been studied and reaction mechanisms have been proposed.
A method for the preparation of trichloroacetyl chloride with silicon tetrachloride (by machine translation)
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Paragraph 0028; 0029; 0030, (2016/11/17)
The invention discloses a method for the preparation of trichloroacetyl chloride with silicon tetrachloride, silicon tetrachloride used as acyl chloride reagent, and trichloro acetic acid in 60-70 °C reaction under 2-4 hours, generating acetic chloride, generated after the cure, the trichloro acetyl chloride and other products by distillation or extraction method for separating. The effective conversion of this invention and an organosilicon polycrystalline silicon production of by-product production in a large amount of silicon tetrachloride, trichlor-production with high added value; in the conversion treatment brought by the development of the production of polycrystalline silicon is difficult to control at the same time the by-product silicon tetrachloride, significantly reduces the cost of the preparation of trichloroacetyl chloride. (by machine translation)
Synthesis, characterization and molecular structures of barium(II) trichloroacetate DME/1,4-dioxane compounds
Singh, Sukhjinder,Saini, Deepika,Mehta,Kaur, Ravneet,Ferretti, Valeria
scheme or table, p. 202 - 209 (2012/03/10)
Two new barium(II) trichloroacetate compounds, [Ba(H2O)(DME) (μ-O2CCCl3)2]n (1) and [{Ba(H2O)2(diox)0.5(μ-O2CCCl 3)2}(diox)]n (2) were synthesized and characterized by elemental analyses, physiochemical studies, FT-IR, 1H NMR, thermogravimetric analyses (TG/DTG/DSC) and single crystal X-ray studies. The reaction of hydrated barium(II) trichloroacetate monohydrate with excess DME (1,2-dimethoxyethane) and diox (1,4-dioxane) in methanol at room temperature led to the isolation of the novel compounds 1 and 2, respectively. Bridging trichloroacetate groups are anticipated on the basis of FT-IR studies and this was confirmed by the X-ray studies. Both compounds dissociate to produce ions in water, as shown by molar conductance values. 1H NMR spectroscopy confirms that DME and 1,4-dioxane are coordinated to the metal ion in these compounds. Single crystal X-ray diffraction studies reveal that the barium cation is coordinated to nine O atoms in a deformed coordination polyhedron in both compounds. Structural data of barium(II) trichloroacetates compounds have been obtained for the first time in the present investigation.
Reaction of carboxylic acids with tetrachlorosilane
Voronkov,Vlasov,Belousova,Grigor'Eva,Vlasova
experimental part, p. 318 - 321 (2010/09/07)
Tetrachlorosilane reacted with carboxylic acids RCOOH (R = Me, Bu, t-Bu) to give the corresponding acid chlorides RCOCl in 75-95% yield. The reactions of SiCl4 with trichloroacetic and 2-fluorobenzoic acids (R = Cl 3C, 2-FC6H4) occurred more difficultly, presumably for steric reasons, and the yields of the corresponding acid chlorides were 11 and 22%, respectively. Tetrachlorosilane failed to react with stearic acid under analogous conditions. Products of the reactions of SiCl 4 with chloroacetic and benzoic acids RCOOH (R = ClCH2, Ph) were tetraacyloxysilanes Si(OCOR)4, and tetrakis(chloroacetoxy) silane was formed in almost quantitative yield. The reaction of SiCl4 with glutaric acid led to the formation of a rubber-like polymeric material with the composition C5H6Cl2O4Si. The effect of pKa values of carboxylic acids on the direction and mechanism of the examined reaction is discussed.
Practical and chemoselective reduction of acyl chloride to alcohol by borohydride in aqueous dichloromethane
Rajan, Ramya,Badgujar, Sachin,Kaur, Kamaljit,Malpani, Yashwardhan,Kanjilal, Pranab R.
experimental part, p. 2897 - 2907 (2010/11/18)
A simple methodology for the reduction of acid chlorides to their corresponding alcohols has been developed. Various carboxylic acids were converted to alcohols in excellent yields using NaBH4-K2CO3 in a mixed solvent system of dichloromethane and water (1:1) in the presence of a phase-transfer catalyst at low temperature. The importance of the work is its simplicity, selectivity, excellent yield, and very short reaction time. This new reduction condition has proved to be an excellent chemoselective method for a range of acid chlorides in the presence of various functional groups.