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Preparation method of high-purity topiramate

A topiramate, high-purity technology, applied in the field of preparation of high-purity topiramate, can solve the problems of poor controllability, limited sources, potential safety hazards and the like

Inactive Publication Date: 2017-05-10
SHAANXI DASHENG PHARMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Sulfamoyl chloride is a highly toxic reagent with limited sources
In addition, the controllability of the whole reaction process is poor, there is a considerable safety hazard, and it cannot be industrialized

Method used

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  • Preparation method of high-purity topiramate
  • Preparation method of high-purity topiramate
  • Preparation method of high-purity topiramate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 17.1 g of sulfuryl chloride and 140 ml of toluene to a 500 ml three-necked flask at room temperature and cool down to -10°C. Add dropwise a mixed solution of 30 g of fructose diacetone, 140 ml of toluene, and 11 g of pyridine. The dropwise addition temperature does not exceed 5° C., and the ice bath is removed after the dropwise addition. The temperature was naturally raised and stirred for 2 hours, and 140 ml of water was added to wash the organic phase. The organic layer was washed successively with 90 ml of 10% hydrochloric acid, 90 ml of purified water, 90 ml of saturated sodium bicarbonate, and 90 ml of saturated sodium chloride. Toluene was distilled off under reduced pressure to obtain 42 g of light yellow oil.

[0033] Dissolve the light yellow oil obtained in the previous step in 300ml tetrahydrofuran, pass ammonia gas at 20-30°C for 5-7 hours, filter off the solid formed by the reaction, rinse the filter cake with 30ml tetrahydrofuran, combine the organic...

Embodiment 2

[0036] Add 17.1 g of sulfuryl chloride and 140 ml of toluene to a 500 ml three-necked flask at room temperature and cool down to -10°C. Add dropwise a mixed solution of 30 g of fructose diacetone, 140 ml of toluene, and 11 g of pyridine. The dropwise addition temperature does not exceed 5° C., and the ice bath is removed after the dropwise addition. The temperature was naturally raised and stirred for 2 hours, and 140 ml of water was added to wash the organic phase. The organic layer was successively washed with 90 ml of 10% hydrochloric acid, 90 ml of purified water, 90 ml of saturated sodium bicarbonate, and 90 ml of saturated sodium chloride. Toluene was distilled off under reduced pressure to obtain 42 g of light yellow oil.

[0037] Dissolve the light yellow oil obtained in the previous step in 300ml tetrahydrofuran, pass ammonia gas at 20-30°C for 5-7 hours, filter off the solid generated by the reaction, rinse the filter cake with 30ml tetrahydrofuran, combine the orga...

Embodiment 3

[0040] Add 17.1 g of sulfuryl chloride and 140 ml of dichloroethane to a 500 ml three-necked flask at room temperature and cool down to -10°C. Add dropwise a mixed solution of 30 g of fructose diacetone, 140 ml of dichloroethane, and 11 g of pyridine. The dropwise addition temperature does not exceed 5° C., and the ice bath is removed after the dropwise addition. The temperature was naturally raised and stirred for 2 hours, and 140 ml of water was added to wash the organic phase. The organic layer was successively washed with 90 ml of 10% hydrochloric acid, 90 ml of purified water, 90 ml of saturated sodium bicarbonate, and 90 ml of purified water. Dichloroethane was distilled off under reduced pressure to obtain 41.5 g of light yellow oil.

[0041] Dissolve the light yellow oil obtained in the previous step in 300ml of dichloroethane, pass ammonia gas at 20-30°C for 7 hours, filter off the solid generated by the reaction, rinse the filter cake with 30ml of dichloroethane, co...

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Abstract

The invention discloses a preparation method of high-purity topiramate. Under the condition of dissolving the topiramate into an organic solvent, a proper concentration of alkali is added, so that the topiramate slat forms solid to be separated out in the solvent; the solid is dissolved into water, and is acidified into a weak acidic state; the solid is a topiramate coarse product; the topiramate coarse product is recrystallized to obtain the high-purity topiramate. The preparation method of the high-purity topiramate has the advantages that the purity reaches 99.90 percent or higher; under the condition that the product purity reaches 99.9 percent or higher, the yield of the product keeps unchanged; no additional excessive cost is added. The operation is convenient; the process is safe; the industrial production is easy.

Description

technical field [0001] The invention provides a preparation method of high-purity topiramate. Background technique [0002] Topiramate is a GABA reuptake inhibitor developed by Johnson & Johnson Pharmaceutical Company of the United States. In 1995, it was launched in the UK as a commodity Topamax, and it is clinically used for the treatment of epilepsy in adults. Topiramate has been listed in more than 60 countries and regions around the world so far. [0003] Topiramate, chemical name: 2,3:4,5-bis-O-(1-methylethylene)-β-D-fructopyranose sulfamate, English name Topiramate, molecular formula: C 12 h 21 NO 8 S, the United States Pharmacopoeia (USP) has been recorded, the structural formula is: [0004] [0005] U.S. Patent No. 4,513,006 provides the following route to prepare topiramate Scheme1: [0006] [0007] The method prepares topiramate by reacting fructose diacetone and aminosulfonyl chloride in the presence of NaH and DMF. Sulfamoyl chloride is a highly to...

Claims

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Application Information

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IPC IPC(8): C07H9/04C07H1/06
CPCC07H9/04C07H1/06
Inventor 薛朝允杨刚利
Owner SHAANXI DASHENG PHARMA TECH
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