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Preparation method of high purity allopurinol sodium

A high-purity sodium allopurinate technology, which is applied in the field of medicine, can solve the problems of low quality controllability of finished products and ineffective removal of by-products of salt-forming reactions, etc., and achieves simple operation, mild reaction conditions and high yield. Effect

Active Publication Date: 2015-08-19
HEFEI JIUNUO MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method introduces impurities into the raw materials, and the by-products of the salt-forming reaction cannot be effectively removed, and all of them will be transferred to the finished preparation, and the quality controllability of the finished product is not high

Method used

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  • Preparation method of high purity allopurinol sodium
  • Preparation method of high purity allopurinol sodium
  • Preparation method of high purity allopurinol sodium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Introduce nitrogen into a 1L four-necked flask, add 160ml of water and 32g of sodium hydroxide, stir to dissolve, control the temperature at 20-30°C, add 100g of allopurinol in batches, stir to dissolve, filter, transfer the filtrate to a 2L four-necked flask, Nitrogen protection, temperature control at 15-25°C, 600ml of acetone was added dropwise within 1h, after dropping, stirred and crystallized for 1h, filtered, washed with an appropriate amount of acetone, the solid was collected, dried under reduced pressure at 140-150°C for 2h, and 95g of white powder was obtained. Yield 81.8%, purity 99.96% (HPLC method).

[0044] Elemental Analysis for C 5 h 3 N 4 Na

[0045] Analysis Project

C（%）

H（%）

N（%）

Na (%)

theoretical value

37.99

1.91

35.44

14.54

measured value

37.91

1.93

35.44

14.55

[0046] TOF-MS[M-Na] + : 135.1

[0047] IR(KBr)ν(cm -1 ): 3199, 3103, 3001, 1595, 1530, 1299

[0048]...

Embodiment 2

[0053] Introduce nitrogen into a 1L four-necked flask, add 400ml of methanol and 40g of sodium methoxide, stir to dissolve, control the temperature at 10-15°C, add 100g of allopurinol in batches, stir to dissolve, filter, transfer the filtrate to a 2L four-necked flask, Under nitrogen protection, temperature control at 15-25°C, 600ml of tetrahydrofuran was added dropwise within 1 hour, after the drop was completed, stirred and crystallized for 1 hour, filtered, washed with a proper amount of acetone, the solid was collected, dried under reduced pressure at 140-150°C for 3 hours, and 92g of white powder was obtained. Yield 79.2%, purity 99.92% (HPLC method).

Embodiment 3

[0055]Introduce nitrogen gas into a 1L four-necked flask, add 500ml of ethanol and 50g of sodium ethoxide, stir to dissolve, control the temperature at 0-10°C, add 100g of allopurinol in batches, stir to dissolve, filter, transfer the filtrate to a 2L four-necked flask, Nitrogen protection, temperature control 15-25°C, dropwise add ethylene glycol dimethyl ether 900ml within 1h, after dropping, stir and crystallize for 1h, filter, wash with ethylene glycol dimethyl ether, collect solid, 140-150°C After drying under reduced pressure for 3 hours, 88 g of white powder was obtained, with a yield of 75.8% and a purity of 99.95% (HPLC method).

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Abstract

The invention discloses a preparation method of high purity allopurinol sodium, under the condition of air isolation, sodium alkali is dissolved in a polar solvent, at the temperature of 30 DEG C or less, allopurinol is added, dissolved, and filtered, the filtrate is added with a precipitant for crystallization and filtration, a solid is dried under reduced pressure at 140-150 DEG C for 2-3 h to obtain the allopurinol sodium. The purity of the allopurinol sodium prepared by the method is greater than 99.9%, the preparation method is simple in process, convenient in operation, high in yield, low in cost, pure in product and more suitable for industrial production.

Description

1. Technical field [0001] The invention relates to a preparation method of a known medicine, in particular to a preparation method of high-purity sodium allopurinate, which belongs to the technical field of medicine. 2. Background technology [0002] Allopurinol sodium (Allopurinonol sodium), the chemical name is 1,5-dihydro-4H-pyrazol[3,4-d]pyrimidine-4-monosodium salt, it is used to treat gout and prevent gouty nephropathy, The sodium salt of allopurinol, an auxiliary treatment drug for episodic hyperuricemia and severe epilepsy, has the following structural formula: [0003] [0004] Allopurinol has poor water solubility and can only be made into oral solid preparations, which is limited in clinical application. If allopurinol is made into sodium salt, it has good water solubility and can be made into injections. In May 1996, allopurinol sodium powder for injection (50mg / bottle, trade name: Aloprim TM ) is listed in the United States for the treatment of patients wit...

Claims

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Application Information

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IPC IPC(8): C07D487/04
CPCC07D487/04
Inventor 吴标凌林应阳戴根来
Owner HEFEI JIUNUO MEDICAL TECH