Loxoprofen sodium synthesis
- Product Name:Loxoprofen sodium
- CAS Number:80382-23-6
- Molecular formula:C15H19NaO3
- Molecular Weight:270.3
68767-14-6
80382-23-6
General procedure for the synthesis of sodium 2-(4-((2-oxocyclopentyl)methyl)phenyl)propionate from 2-(4-((2-oxocyclopentyl)methyl)phenyl)propionic acid: 2-(4-((2-oxocyclopentyl)methyl)phenyl)propionic acid and methanol were added into a round-bottomed flask, and 1 equivalent of aqueous sodium hydroxide was added to the above solution drop by drop, and the reaction was stirred for 1 hour at room temperature. Upon completion of the reaction, a decompression distillation was carried out at 50-55°C to remove the solvent. Subsequently, a 5% aqueous solution of ethyl acetate was added to the residue, heated until dissolved and then slowly cooled to room temperature. Crystallization was induced by the addition of crystal seeds during cooling and stirring was continued for 5-6 hours at 0-5°C until a suspension was formed. Finally, the solid was collected by filtration to give loxoprofen sodium dihydrate in 95% yield and 99.1% HPLC purity.
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80382-23-6
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Yield:80382-23-6 35.36 g
Reaction Conditions:
with sodium hydroxide in ethanol; for 1 h;Reflux;
Steps:
16 Preparation of loxoprofen sodium
Methyl 2-(4-((2-oxocyclopentyl)methyl)phenyl) propionate (compound 6, 38 g, 154.28 mmol) was introduced into a 500 ml three-necked flask, ethanol (200 ml) was added, refluxed, and sodium hydroxide solution (20.9 g, 30% by mass) was dropped to the resulting mixture for 1 hour. After completion of dripping, the material was concentrated to dryness. The residue was recrystallized from ethanol-methyl tert-butyl ether to give a white powdery solid (35.36 g, 131.80 mmol). Molar yield 85.43%, HPLC purity 99.7%
References:
CN106699559,2017,A Location in patent:Paragraph 0116-0118
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