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Preparation method of arginine dexibuprofen

A technology of dextrobuprofen and arginine, which is applied to the preparation of organic compounds, chemical instruments and methods, separation/purification of carboxylic acid compounds, etc., can solve the problem of poor control of dropping speed and flow rate, poor reaction, etc. Complete, related substances and other issues, to achieve the effect of correcting liver toxicity, increasing supply, and high product purity

Active Publication Date: 2012-02-08
HAINAN HULUWA PHARMA GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method is to use L-arginine aqueous solution-200ml ethanol dropwise, it is not easy to control the speed and flow rate of dropping, and adopts reaction at room temperature for 1h, 0 ℃ insulation for 2h, at this temperature, first react the arginine produced Dexibuprofen will be precipitated, resulting in incomplete final reaction, resulting in high related substances and low yield in the final product

Method used

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  • Preparation method of arginine dexibuprofen
  • Preparation method of arginine dexibuprofen

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Dissolve 20.83g (0.101mol) of Dexibuprofen in 72ml of 95% (volume percent concentration) ethanol aqueous solution, heat to 55°C, and slowly and continuously add 17.42g (0.1mol) of L-arginine dropwise under stirring, After 10 minutes of dropwise addition, keep stirring at 55°C for 3 hours, let stand for 30 minutes, then cool to room temperature, filter with suction to obtain crystals, wash 3 times with 5ml of 95% (volume percent concentration) ethanol aqueous solution, and dry at 65°C for 6 hours to obtain white The crystal is 37.66g, the yield is 98.98%, and the melting point is 175°C-178°C.

[0035] The above-mentioned white crystals were subjected to elemental analysis, and the results of the main components were as follows: C: 60.04%, H: 8.51%, N: 14.71% (both by mass percentage), and the theoretical value of arginine Dexibuprofen: C: 59.97 %, H: 8.47%, N: 14.71% (both mass percentages) are consistent. It shows that the main component of the above product is D-α-met...

Embodiment 2

[0037] Dissolve 22.12g (0.107mol) of Dexibuprofen in 72ml of 95% (volume percent concentration) ethanol aqueous solution, heat to 50°C, and slowly and continuously add 17.42g (0.1mol) of L-arginine dropwise under stirring, After 15 minutes of dropwise addition, keep stirring at 50°C for 2 hours, let stand for 25 minutes, then cool to room temperature, filter with suction to obtain crystals, wash 3 times with 5ml of 95% (volume percent concentration) ethanol aqueous solution, and dry at 70°C for 4 hours to obtain white The crystal is 37.46g, the yield is 98.45%, and the melting point is 175.2°C-177.6°C.

[0038]The above-mentioned white crystals were subjected to elemental analysis, and the main component results were as follows: C: 60.12%, H: 8.48%, N: 14.77% (both by mass percentage), and the theoretical value of arginine Dexibuprofen: C: 59.97 %, H: 8.47%, N: 14.71% (both mass percentages) are consistent. It shows that the main component of the above product is D-α-methyl-4...

Embodiment 3

[0040] Dissolve 21.94g (0.106mol) of Dexibuprofen in 72ml of 95% (volume percent concentration) ethanol aqueous solution, heat to 60°C, and slowly and continuously add 17.42g (0.1mol) of L-arginine dropwise under stirring, After 20 minutes of dropwise addition, keep stirring at 60°C for 3.5 hours, let stand for 35 minutes, then cool to room temperature, filter with suction to obtain crystals, wash 3 times with 5ml of 95% (volume percent concentration) ethanol aqueous solution, and dry at 68°C for 5 hours to obtain 36.86 g of white crystals, the yield is 96.88%, and the melting point is 175.8°C to 178.2°C.

[0041] The above-mentioned white crystals are subjected to elemental analysis, and the main component results are as follows: C: 60.08%, H: 8.49%, N: 14.77% (both by mass percentage), and the theoretical value of arginine dextroibuprofen: C: 59.97 %, H: 8.47%, N: 14.75% (both mass percentages) match. It shows that the main component of the above product is D-α-methyl-4-(2-...

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Abstract

The invention discloses a preparation method of an arginine dexibuprofen raw medicine. The method comprises the steps of: dissolving dexibuprofen in ethanol, heating the mixture to a temperature of 50DEG C-60DEG C, adding L-arginine in a dropwise manner slowly and continuously under stirring within 10min-20min, continuing stirring for reaction for 2h-3.5h with the temperature maintained at 50DEG C-60DEG C, leaving the mixture to stand for 25min-35min and cool to a temperature of 18DEG C-30DEG C, conducting pumping filtration so as to obtain crystals, then washing and drying the crystals, thus obtaining white crystals, i.e. arginine dexibuprofen. The preparation method of the invention has simple process, high yield, no refining step, shortened production period, and no need for any special equipment, thus being suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of raw material medicine preparation, in particular to a method for preparing arginine-dextroibuprofen raw material medicine. Background technique [0002] The chemical name of Arginine Dexibuprofen: D-α-methyl-4-(2-methylpropyl)phenylacetic acid L-2-amino-5-guanidinovalerate, the chemical structure is: [0003] [0004] Molecular formula: C 13 h 18 o 2 ·C 6 h 14 N 4 o 2 , molecular weight: 380.48. [0005] Ibuprofen is a representative drug among non-steroidal anti-inflammatory drugs. It has anti-inflammatory, antipyretic and analgesic effects. The main product in pyretic analgesics has replaced aspirin as the most commonly used antipyretic analgesic. [0006] But ibuprofen solubility is little, in order to solve the problem that ibuprofen has little solubility in water and low melting point preparation difficulty, ibuprofen and arginine are made organic salt abroad, can obtain crystalline solid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C57/30C07C51/42C07C279/14C07C277/08A61P3/02A61P39/02A61P37/02
Inventor 刘全国陈克领
Owner HAINAN HULUWA PHARMA GRP CO LTD
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