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Preparation method of denufosol tetrasodium

A technology of dinufosol and nufosol sodium, applied in the field of medicine and chemical industry, can solve the problems of large energy loss, complicated steps, inconvenient operation and the like

Active Publication Date: 2020-06-09
GUANGDONG XIANQIANG PHARMA +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Alternative elution using cation exchange columns and anion exchange columns can effectively remove high molecular weight impurities, but a large amount of water will be generated during the elution process, and there are certain requirements for equipment in production, which is inconvenient to operate, so it needs a A more convenient method to replace the traditional cation exchange column and anion exchange column alternate elution method, so as to overcome the problems of complex steps and large energy loss in the preparation process of denufosol sodium

Method used

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  • Preparation method of denufosol tetrasodium
  • Preparation method of denufosol tetrasodium
  • Preparation method of denufosol tetrasodium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] The following steps are used to refine Nufosol Sodium:

[0038] a) Add 100g of denufosol crude product (purity above 90%) into 700ml of N,N-dimethylformamide, after dissolving, prepare 53.0g of sodium acetate as a saturated aqueous solution and add to the above system, heat to 60°C, After 2 hours of salt formation reaction, 1400ml of ethanol was added, the temperature was lowered to 0°C for crystallization, and 99.8g of crude product of denufosol sodium was obtained by filtration;

[0039] b) Add the crude product of denufosol sodium to 700ml of water, use concentrated hydrochloric acid to adjust the pH to 2.5, add 1.3g of calcium chloride and stir to dissolve, then add 50% aqueous sodium hydroxide solution dropwise to adjust the pH to 6-7, filter and heat After reaching 50°C, 1500ml of methanol solution was added for crystallization to obtain 97.5g of denufosol sodium refined product with a yield of 87.7% and a purity of 99.3%.

[0040] Yield % = Denufosol Sodium Fine M...

Embodiment 2～7 and comparative example 1～4

[0042] Examples 2-7 and Comparative Examples 1-4 are the same as Example 1 in terms of feeding and operating methods. Reactants, reaction conditions and yield and purity are shown in Table 2.

[0043] Table 2 embodiment 2~7 and comparative example 1~4 experimental conditions and result

[0044]

[0045]

[0046] As can be seen from the data in Table 2, when the calcium salt used in the preparation method described in Example 1 is calcium chloride, the yield and purity are higher, and when the preparation method described in Comparative Example 3 uses magnesium chloride, the magnesium salt and phosphoric acid impurities The incorporation rate is relatively low, therefore, the obtained Denufosol Sodium boutique purity is lower. It can be seen from Comparative Example 2 and Comparative Example 4 that too high or too low sodium salt dosage is not conducive to the formation of denufosol sodium salt. As can be seen from Comparative Example 1 and Comparative Example 2, the am...

Embodiment 8

[0048] Using the above-mentioned Examples 1-3, Comparative Examples 1-3 and Denufosol Sodium prepared according to the patent ZL200780028646.9 as raw materials, and prepare Denufosol Sodium Eye Drops with the same prescription. Sona Eye Drops was inspected at 25°C for 3 months, and the number of particles of 10 μm and above and the number of particles of 25 μm and above in each container (part) of the test product were detected and recorded by the insoluble particle photoresist method of the General Rules of the Chinese Pharmacopoeia (0903) The results are shown in Table 3.

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Abstract

The invention discloses a refined preparation method of denufosol tetrasodium. The refined preparation method comprises the steps of after preparing salt through a specific reaction organic solvent and sodium salt, adding specific calcium salt, filtering impurities, and performing crystallization in a specific organic solvent so as to obtain high-purity denufosol tetrasodium quality products. Theprepared denufosol tetrasodium is used for preparing a preparation, and after the preparation is kept for a long time, phenomena of precipitation and turbidity are not generated.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry. Specifically, the invention relates to a method for refining denufosol sodium. Background technique [0002] Denufosol sodium (Denufosol tetrasodium), CAS number: 318250-11-2, chemical name P 1 -(2'-deoxycytidine 5'-)P 4 -(Uridine 5'-)tetraphosphate Tetrasodium 2'-deoxycytidine(5')tetraphospho(5')uridinetetrasodium, the chemical formula is as follows: [0003] [0004] Dinufoso is a P2Y 2 Receptor agonists, by acting on P2Y 2 Receptor goblet cells of the membrane and conjunctival epithelial cells, thereby increasing the concentration of intracellular calcium ions, promoting the secretion of mucin and water, and improving corneal epithelial disorders. In addition, it can also be used to treat sinusitis, otitis media, nasolacrimal duct blockage, dry eye disease and retinal detachment. [0005] At present, there are few reports about the preparation method of denufosol...

Claims

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Application Information

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IPC IPC(8): C07H21/04C07H1/00C07H1/06
CPCC07H1/00C07H1/06C07H21/04
Inventor 谭珍友邓军叶琼仙刘道甫钟颖强
Owner GUANGDONG XIANQIANG PHARMA
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