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Preparation method for improving pamabrom refining yield and purity

A technology of yield of pamabromide and bromine, applied in the field of medicine, can solve problems such as poor uniformity, unfavorable drying, etc., and achieve the effects of reducing the amount of solvent, being beneficial to later drying, and loosening the crystal form

Inactive Publication Date: 2016-10-12
BEIJING CHENG JI PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present inventor refines the crude product Pamabromide according to the above-mentioned preparation method, and the resulting product is block, and the yield is only about 30%, which is unfavorable for drying and has poor uniformity.

Method used

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  • Preparation method for improving pamabrom refining yield and purity
  • Preparation method for improving pamabrom refining yield and purity
  • Preparation method for improving pamabrom refining yield and purity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] According to the refining method of Pamabromide described in Chinese patent CN200910172351:

[0024] Take 140g of crude product Pamabromide, put it into a 1000mL three-necked flask, add 240g of ethanol and 40g of the mixture, stir to dissolve, heat up to 50°C, add activated carbon, continue to stir for 20min, filter while it is hot, stand for crystallization, filter, 30g without Washed with water and ethanol, and dried under vacuum to obtain 43.5 g of the product, with a yield of 31.1%.

Embodiment 2

[0026] A kind of preparation method that improves the yield and purity of Pamabromide refining provided by the invention 1

[0027] Take 200g of crude product Pamabromide, add it to a 1000mL three-neck flask, add 10g of water, 300g of ethanol, heat up to 55°C, stir to make it completely dissolved, continue to stir for 15min, filter while it is hot, and naturally cool the filtrate to 15- Continue to stir and crystallize at 20°C for 3h, then stand still for 12h, filter, wash the filter cake with 50g of absolute ethanol, and vacuum-dry the filter cake to obtain 168.6g of pure Permabromide with a purity of 99.99% and a yield of 84.3%.

Embodiment 3

[0029] A kind of preparation method that improves the refining yield and purity of Pamabromide provided by the invention 2

[0030] Take 800g of crude product Pamabromide, add it to a 5000mL three-necked flask, add 40g of water, 1200g of ethanol, heat up to 55°C, stir to make it completely dissolved, continue to stir for 15min, filter while it is hot, and naturally cool the filtrate to 15- Continue to stir and crystallize at 20°C for 3 hours, then stand for crystallization for 12 hours, filter, wash the filter cake with 50 g of absolute ethanol, and vacuum-dry the filter cake to obtain 676.0 g of pure Permabromide with a purity of 99.99% and a yield of 84.5%.

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Abstract

Belonging to the field of medical technology, the invention in particular relates to a preparation method for improving pamabrom refining yield and purity. By controlling the proportion of alcohol and a water solvent, the crystallization temperature and other critical processes and parameters, the method prepares high purity pamabrom with yield of greater than 80% and purity of more than 99.9%. The alcohol is ethanol, methanol or isopropanol, preferably ethanol, the dosage of ethanol is 1.4-1.6 times the mass of crude pamabrom, the dosage of water is 0.4-0.6 times the mass of the crude pamabrom, and the crystallization temperature is 15-20DEG C. The method provided by the invention effectively solves the technical problems of low pamabrom refining yield and low purity, and has the advantages of simple process, good reproducibility, low cost, environmental protection and energy saving, etc., thus having high clinical value and significant social and economic benefits. The pamabrom provided by the invention is used for treatment of headache, breast swelling, lower limb edema and other menstrual syndromes caused by swelling and water retention in menstrual period.

Description

technical field [0001] The invention belongs to the technical field of medicines, and in particular relates to a preparation method for improving the refining yield and purity of Pamabromide. The preparation method is to control the ratio of alcohol and water solvent, dissolution temperature, stirring time, crystallization temperature and crystallization time and other processes and parameters, thereby preparing high-purity Pa horse bromide. Background technique [0002] Pama bromide, English name Pamabrom, its chemical name is: 8-bromo-3,7-dimethyl-1H-purine-2,6-diketone-2-amino-2-methyl-1-propanol, Molecular formula: C 11 h 18 BrN 5 0 3 , molecular weight: 348.20, structural formula: [0003] [0004] Chinese patent CN200910172351 discloses a refined preparation method of Pamabromide: add crude Pamabromide into a reaction vessel, then add ethanol with a volume percentage concentration of 75-90%, heat to 50-55°C, stir to dissolve, and add activated carbon , stirre...

Claims

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Application Information

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IPC IPC(8): C07D473/08
CPCC07D473/08
Inventor 张凯魏科伟童丰陈永建
Owner BEIJING CHENG JI PHARMA
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