80382-23-6Relevant articles and documents
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.
Loxoprofen sodium preparation method
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Paragraph 0022-0029, (2019/05/11)
The invention discloses a loxoprofen sodium preparation method, which comprises: directly carrying out alkylation on 2-(p-bromomethyl)isophenylpropionic acid as a starting raw material under a NaOH and DMF system, carrying out hydrolysis decarboxylating to obtain a crude product, separating the by-product produced in the reaction through high-vacuum distillation to obtain loxoprofen acid, and carrying out salt forming to obtain the loxoprofen sodium. According to the present invention, the method has characteristics of less synthesis step, mild reaction condition, reasonable price and easy purchase of the raw material, low pollution and low production cost, and is suitable for industrial production, wherein the product content can reach more than 99.8%, and the single impurity is less than0.05%.
Loxoprofen sodium dihydrate crystal form and preparation method thereof
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Paragraph 0034-0041, (2019/01/10)
The invention relates to a loxoprofen sodium dihydrate crystal form preparation method thereof. The loxoprofen is dissolved in a dissolving solvent and reacted with sodium-containing base to prepare loxoprofen sodium, and after adding water, the seed crystal may or may not be added to prepare the loxoprofen sodium dihydrate crystal form. The crystal form preparation method obtains the high-puritycrystal form, and the novel crystal form has good fluidity and appearance.