68767-14-6Relevant articles and documents
Synthetic method of loxoprofen
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Paragraph 0034; 0083; 0089-0090; 0095; 0100-0101, (2020/08/02)
The invention discloses a synthetic method of an intermediate loxoprofen for preparing a phenylpropionic acid non-steroidal anti-inflammatory drug loxoprofen sodium. The synthetic method comprises thefollowing steps: firstly, carrying out acylation reaction on a compound VII and a compound VIII in a solvent 1 under the action of lewis acid serving as a catalyst to obtain an intermediate compoundIX; and introducing hydrogen into the intermediate compound IX in a solvent 2 under the action of strong acid by taking palladium on carbon as a catalyst, and carrying out hydrogenation tert-butyl ester removal reaction to obtain loxoprofen. The synthetic method has the advantages that the synthetic route is short, simple in process and convenient to operate, no corrosive strong acid is used in the synthesis process, and the reaction control temperature in the synthesis process is relatively mild; and the synthetic method has the characteristics of no product carbonization, no corrosion to equipment, safe and environment-friendly synthesis process, suitability for industrial production and the like, and the finally obtained product loxoprofen has high yield which can reach 65.8-73.3% and purity of 99.54-99.69% from the beginning of the compound VIII.
Preparation method of aryl propionic acid compound
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Page/Page column 0121-0125, (2020/10/04)
The invention provides a preparation method of an aryl propionic acid compound, wherein the preparation method comprises the following steps: carrying out acetylation reaction on substituted aryl benzene to obtain aryl acetophenone; carrying out hydrogenation reduction reaction on alpha-substituted aryl ethyl ketone to obtain alpha-substituted aryl ethanol; and in an acidic solution, introducing carbon monoxide gas into the alpha-substituted aryl ethanol, and carrying out a carbonylation reaction under the co-catalytic action of a main catalyst and a cocatalyst to obtain the aryl propionic acid compound, wherein the cocatalyst has the following structural formula described in the specification, R1 is one of hydrogen and a substituted carboxylic acid group, and R2 is one of hydrogen, halogen, substituted or unsubstituted C1-C12 alkyl, substituted or unsubstituted C1-C6 alkoxy, substituted or unsubstituted C3-C12 naphthenic base, substituted carbonyl containing C6-C24 aryl or substitutedaryl, substituted carbonyl containing C3-C12 heterocyclic radical or substituted heterocyclic radical, phenyl, substituted phenyl, naphthyl and substituted naphthyl.
Synthesis method of loxoprofen sodium
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, (2019/06/07)
The invention discloses a synthesis method of loxoprofen sodium, which comprises the following steps of: step 1), preparing N-(1-cyclopentenyl) morpholine; step 2), preparing 2-(4-bromomethyl phenyl)methyl propionate, the method also comprises the following step 3), preparing loxoprofen sodium by an enamine alkylation method: first dissolving 2-(4-bromomethyl phenyl) methyl propionate in a solvent, adding N-(1-cyclopentenyl) morpholine and the solvent in a container, dropwise adding 2-(4-bromomethyl phenyl) methyl propionate solution under reflux conditions; continuing reacting under reflux conditions after the completion of the dropwise addition; adding alkali solution after obtained reaction liquid is cooled, hydrolysising and separating to obtain an organic phase and an aqueous phase respectively, extracting the aqueous phase with an extractant to obtain extract liquid and the aqueous phase after extraction respectively, and post-treating the aqueous phase after extraction to obtain loxoprofen sodium. The preparation of loxoprofen sodium by the above method has the advantages of simple reaction steps, high yield of loxoprofen sodium and low production cost.
