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Medicinal disodium creatine phosphate hexahydrate and preparing method thereof

A technology of creatine phosphate disodium salt and hexahydrate, which is applied in the field of pharmaceutical creatine phosphate disodium salt hexahydrate and its preparation, which can solve the impact on product quality, affect the clarity inspection of injections, and the results cannot meet the regulations, etc. Problems, to achieve good fluidity, avoid thermal decomposition, easy to dry the end of the effect

Active Publication Date: 2007-09-12
QIDONG HUATUO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Inorganic salt impurities have a significant impact on product quality. For example, creatine phosphate disodium salt injection for final intravenous injection, when the product contains more than 1.5% inorganic phosphate (calculated as disodium hydrogen phosphate) by weight, according to the "China During the abnormal toxicity inspection of the second appendix of the Pharmacopoeia of the People's Republic of China in 2005, the results did not meet the requirements; in addition, inorganic salt impurities also affected the clarity inspection of injections

Method used

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  • Medicinal disodium creatine phosphate hexahydrate and preparing method thereof
  • Medicinal disodium creatine phosphate hexahydrate and preparing method thereof
  • Medicinal disodium creatine phosphate hexahydrate and preparing method thereof

Examples

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Effect test

Embodiment 1

[0034] Embodiment 1: the preparation of creatinine chlorinated phosphoric acid

[0035]In a 250ml round bottom flask, put 5.0g of creatinine and 150ml of re-evaporated and dried POCl 3 . Heat to reflux under stirring for 15 minutes, then lower the temperature to 80°C, and distill out about 135ml of POCl under reduced pressure 3 , add 20ml of toluene to the remaining yellow viscous liquid, cool to room temperature under stirring, filter, and wash the filter cake with a small amount of solvent to obtain about 10g of creatinine phosphorus oxychloride with a melting point of 120-123°C.

Embodiment 2

[0036] Embodiment 2: the preparation of creatinine chlorinated phosphoric acid

[0037] In the 500L reactor, pump POCl 3 360L, creatinine 12Kg, stirred and heated to reflux for 1 hour, dissolved, cooled to 80°C and evaporated under reduced pressure to remove POCl 3 , to 40-50Kg, add 50kg of toluene, cool to room temperature, precipitate crystals, filter, wash with a small amount of toluene, and drain to obtain creatinine chloride with a wet weight of about 20kg. The melting point is 120-123°C.

Embodiment 3

[0038] Embodiment 3: Preparation of creatine phosphate disodium salt crude product

[0039] Add 160ml of 4mol / l NaOH solution into a 500ml round bottom flask, cool to -5°C with an ice-salt bath, and slowly add 36g of creatinine chloride prepared in Example 2. The solid dissolved slowly, and kept stirring at about 0°C for 1 hour until the reaction system no longer exothermic, then raised the temperature to 45°C, and stirred for 12 hours. Cool to room temperature, adjust pH to 8.0-9.0 with concentrated hydrochloric acid, slowly add 40ml of ethanol, filter, add 600ml of ethanol to the filtrate, let it stand for 12 hours, white crystals precipitate, filter, and dry to obtain 26g of crude creatine phosphate disodium salt.

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Abstract

This invention discloses a phosphocreatine disodium salt six-hydrate and its preparation method. The compound is phosphocreatine disodium salt with high purity and six-crystal water, and the preparation method includes the following steps: (1) Kondens of creatinine and phosphorus oxychloride prepares creatinine phosphorus oxychloride, (2) creatinine phosphorus oxychloride is taken the ring opening reaction to get crude phosphorus disodium, (3) purification and crystallization gets the target product. This invention has the advantages of high purity suitable for the manufacture of injection powder, and it avoids the large use of solvents with high yield of products. The excessive phosphorus oxychloride is reused with distillation, and the product has high purity through intermediate and resin purification. It has no potential safety problem about heavy metal residues, and can effectively improve the clarification to reach the intravenous requirement.

Description

technical field [0001] The invention relates to a medicinal creatine phosphate disodium salt hexahydrate and a preparation method thereof. Background technique [0002] Creatine phosphate disodium salt is a metabolic cardioprotective and therapeutic drug. The current classic method for the synthesis of creatine phosphate disodium salt is to use creatine as the starting material, and drop phosphorus oxychloride in aqueous sodium hydroxide solution. Condensation, barium or calcium salt exchange purification to get creatine phosphate disodium salt. This is a conventional method for preparing creatine phosphate disodium salt of reagent specification. React in sodium hydroxide solution and add excess phosphorus oxychloride. There are a large amount of unreacted creatine and inorganic phosphate in the reaction system, so it can only be used After barium salt exchange and purification, ethanol or methanol is added to the aqueous solution for crystallization to obtain products with...

Claims

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Application Information

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IPC IPC(8): C07F9/22
Inventor 吕伟张秋华朱勤韩宇东孙珏郁云忠张德馨李若海潘俊芳
Owner QIDONG HUATUO PHARMA
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