209995-38-0Relevant articles and documents
Preparation method of 2,4,5-trifluorophenylacetic acid
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, (2021/05/29)
The invention belongs to the technical field of preparation of drug intermediates, and discloses a preparation method of 2,4,5-trifluorophenylacetic acid, wherein the preparation method comprises the steps: step 1, reacting raw materials, a quaternary ammonium salt catalyst, sulfolane and potassium fluoride to obtain a first intermediate; step 2, carrying out hydrogenation catalytic reaction on the first intermediate to obtain a second intermediate; step 3, carrying out salt forming reaction on the second intermediate and a fluorinating reagent, quenching, and carrying out diazotization reaction on the second intermediate and a sodium nitrite aqueous solution to obtain diazonium salt; step 4, carrying out high-temperature cracking on the diazonium salt, to obtain 2,4,5-trifluorotoluene; and step 5 to step 7, carrying out halogenation, cyanidation and hydrolysis reactions on 2,4,5-trifluorotoluene in sequence, and thus obtaining 2,4,5-trifluorophenylacetic acid. The raw materials adopted by the method are easy to obtain and low in cost, the yield of the corresponding product obtained in each step is high, and large-scale production of the 2,4,5-trifluorophenylacetic acid is facilitated.
Novel preparation method of 2, 4, 5-trifluorophenylacetic acid
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, (2021/06/23)
The invention discloses a novel preparation method of 2, 4, 5-trifluorophenylacetic acid, which belongs to the technical field of preparation of medical intermediates, and comprises the following preparation steps: carrying out nitration reaction on sulfuric acid and m-dichlorobenzene to obtain an intermediate II; adding the intermediate II, a phase transfer catalyst and potassium fluoride into an aprotic solvent to obtain an intermediate III; performing hydrogenation reaction on the intermediate III to obtain an intermediate IV; carrying out diazotization reaction on the intermediate IV, nitrosyl sulfuric acid and sodium fluoborate to obtain an intermediate V; performing cracking reaction on the intermediate V to obtain an intermediate VI; carrying out reduction reaction on the intermediate VI, and then carrying out bromination reaction on the intermediate VI and liquid bromine to obtain an intermediate VII; subjecting the intermediate VII to a substitution reaction with diethyl malonate, and obtaining 2, 4, 5-trifluorophenylacetic acid after hydrolysis and purification. A novel synthesis route is provided, the problem that technological operation is tedious is solved, the requirements for reaction and operation conditions are low, anhydrous and oxygen-free reaction conditions are not needed, the method is suitable for industrial production, and the yield and purity are greatly improved.
Synthesis method of sitagliptin intermediate 2,4,5-trifluorophenylacetic acid
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Paragraph 0145-0148, (2020/06/09)
The present invention provides a synthesis method of a sitagliptin intermediate 2,4,5-trifluorophenylacetic acid. The method comprises a substitution reaction, a hydrolysis reaction and a decarboxylation reaction, and specifically comprises: A, carrying out a substitution reaction on a compound 4, or sequentially carrying out a substitution reaction and a hydrolysis reaction to prepare a compoundrepresented by a formula 5; B, carrying out a hydrolysis reaction on the compound represented by the formula 5 to prepare a compound represented by a formula 6; and C, carrying out a decarboxylation reaction on the compound represented by the formula 6 under the catalysis of a catalyst to prepare 2,4,5-trifluorophenylacetic acid, wherein the catalyst is a metal oxide. According to the synthesis process, the 2,4,5-trifluorophenylacetic acid compound is prepared with low cost and high yield, and the industrial scale-up production applicability is high.