- Method for preparing aromatic carboxylic acid compound
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The invention discloses a method for preparing an aromatic carboxylic acid compound. The method comprises the following steps: 1) heating carbon dioxide and hydrosilane in the presence of a copper catalyst in a reaction medium A; and 2) adding a reaction medium B, aryl halide, a palladium catalyst and a base to the reaction mixture in the step 1), sealing the reaction system, and performing a heating reaction. The method has the advantages that raw materials are simple and easy to obtain, the raw materials are cheap and stable, the catalyst is common, easy to obtain and stable, the reaction conditionsaremild, the aftertreatment is simple, the yield is high, and the like.
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Paragraph 0141-0143; 0162-0164; 0177
(2020/02/14)
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- Method for preparing aldehyde and acid by electrochemical dehydrochlorination of polychloromethylpyridine derivatives
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The invention discloses a method for preparing aldehyde and an acid by electrochemical dechlorination of a polychloromethylpyridine derivative, the method comprises the following steps: dissolving thepolychloromethylpyridine derivative in an acetic acid and acetate- containing buffer solution to obtain an electrolytic reaction solution; taking the electrolytic reaction solution as a cathode liquid, performing electrolytic reduction dechlorination reaction at a cathode, and hydrolyzing in the solution to obtain a polychlorinated pyridylaldehyde or acid derivative. The polychloromethylpyridinederivative is shown in formula (I), and the product polychlorinated pyridylaldehyde or acid derivative is shown in formula (II): in the formula (I), m is 0, 1, 2, 3 or 4, n is 0 or 1, and R' is an easy-to-oxidize or easy-to-hydrolyze substituent. The m and the R' in the formula (II) are same as that in the formula (I), R is H or OH, no waste acid is generated in the preparation process, the easy-to-oxidize or easy-to-hydrolyze substituent contained in the polychloromethylpyridine derivative and carbon-chlorine bonds on pyridine rings are not affected, and the recovery conversion rate is high.
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Paragraph 0035-0037; 0057-0060
(2020/08/27)
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- Preparation method of 6-amino-2-picolinic acid
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The invention relates to the technical field of organic synthesis, and specifically relates to a preparation method of 6-amino-2-picolinic acid. The preparation method comprises the following steps: taking 2-methyl-6-chloropyridine, potassium permanganate and amino methanol as raw materials; carrying out oxidation, ammonolysis and other reactions, and carrying out purification to obtain high purity 6-amino-2-picolinic acid. The preparation method has low equipment requirements, the operation of the whole process is simple, the synthesis route is short, the byproducts are few, the corrosion islow, the environmental pollution is low, the synthesis method is suitable for industrial production, the structure of the final product is stable, and the content is high.
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Paragraph 0028-0033
(2020/07/15)
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- Tandem one-pot CO2 reduction by PMHS and silyloxycarbonylation of aryl/vinyl halides to access carboxylic acids
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The present study discloses the synthesis of aryl/vinyl carboxylic acids from Csp2-bound halides (Cl, Br, I) in a carbonylative path by using silyl formate (from CO2 and hydrosilane) as an instant CO-surrogate. Hydrosilane provides hydride for reduction and its oxidation product silanol serves as a coupling partner. Mono-, di-, and tri-carboxylic acids were obtained from the corresponding aryl/vinyl halides.
- Paridala, Kumaraswamy,Lu, Sheng-Mei,Wang, Meng-Meng,Li, Can
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supporting information
p. 11574 - 11577
(2018/10/31)
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- Method for preparing picolinafen
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The invention discloses a method for preparing picolinafen, and belongs to the field of pesticide original medicine technology. The method comprises the following steps that (1) 2-chlorine-6-nitrapyrin serves as a raw material, and acid catalysis hydrolysis is carried out to synthesize 2-chlorine-6-pyridine carboxylic acid; (2) under conditions of alkali 1, catalyst and organic solvent 1, etherification reaction is carried out on 2-chlorine-6-pyridine carboxylic acid and m-trifluoromethylphenol to obtain 2-(3-trifluoromethylphenoxy pendant)-6-picolinic acid; (3) the 2-(3-trifluoromethylphenoxypendant)-6-picolinic acid and di(trichloromethyl) dimethyl carboxylate are reacted in alkali 2 and organic solvent 2 to synthesize intermediate 2-(3-trifluoromethylphenoxy pendant)-6-pyridinecarbonylchloride; (4) the intermediate 2-(3-trifluoromethylphenoxy pendant)-6-pyridinecarbonyl chloride and 4-fluoroaniline are reacted in alkali 3 and organic solvent 2 to prepare the picolinafen. The method for preparing the picolinafen has the advantages that the content of the prepared picolinafen product is 98.1%, the yield of the prepared picolinafen product is 83%, synthesis conditions are mild and safe, the operation process is controlled easily, aftertreatment is simple and convenient, the wastewater quantity is less, and the method is a green synthetic method for preparing the picolinafen.
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Paragraph 0011; 0026; 0027
(2018/10/19)
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- Preparation method of 2-substitured phenoxy-6-pyridine formyl chloride and preparation method for picolinafen
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The invention provides a preparation method of 2-substitured phenoxy-6-pyridine formyl chloride and a preparation method for picolinafen. Bis(trichloromethyl) carbonic ester(triphosgene) is used as achloride agent for performing a chloroformylation reaction of 2-(3-trifluoromethylphenoxy)-6-pyridine carboxylic acid. The method is mild in synthesis condition, safe, easy to control an operating process, simple and convenient in post-processing, little in wastewater quantity, and environmentally friendly, and capable of avoiding using corrosive reactants of thionyl chloride and the like, reducing the emission of pollution gases of sulfur dioxide and hydrogen chloride and the like and the emission of wastewater, reducing the requirements to a device, and simplifying the operation, the preparation method is beneficial to improve a preparation method of a picolinafen herbicide, and has the extensive application prospect.
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Paragraph 0031; 0035; 0039
(2018/12/05)
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- Heteroaryl hydroxycarbonylation: An efficient, robust, practically scalable approach using formyl acetate as the co source
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A simple, efficient, regioselective, and scalable palladium-catalyzed hydroxycarbonylation of heteroaryl halides to corresponding carboxylic acids using acetic-formic anhydride in presence of Pd(OAc)2, dppf, and diisopropylethyl amine in dimethyl formamide at 80-90 °C in excellent yields. Taylor & Francis Group, LLC.
- Gadakh, Amol V.,Chikanna, Dinesh,Rindhe, Sahebrao S.,Karale, Bhausaheb K.
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experimental part
p. 658 - 666
(2011/12/16)
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- ARYL-QUINAZOLINE/ARYL-2AMINO-PHENYL METHANONE DERIVATIVES
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A compound of formula (I): wherein R1, R2, R3 and Y are as defined herein, or a pharmaceutically-acceptable and -cleavable ester, or acid addition salt thereof, useful for promoting the release of parathyroid hormone, e.g. for preventing or treating bone conditions which are associated with increased calcium depletion or resorption or in which stimulation of bone formation and calcium fixation in the bone is desirable.
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Page/Page column 123-124
(2008/06/13)
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- Synthesis and analgesic activity of some side-chain modified anpirtoline derivatives
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New derivatives of anpirtoline and deazaanpirtoline modified in the side chain have been synthesized, The series includes compounds 3 with side-chains containing piperidine or pyrrolidine rings, compounds 4 containing 8- azabicyclo[3.2.1]octane moiety, an
- Radl, Stanislav,Hezky, Petr,Proska, Jan,Hejnova, Lucie,Krejci, Ivan
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p. 107 - 112
(2007/10/03)
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