Method for preparing high-purity docusate sodium

A kind of docusate sodium, high-purity technology, applied in the field of preparation of high-purity docusate sodium, can solve the problem of not being able to obtain pure docusate sodium and the like

Active Publication Date: 2012-10-03
HUNAN WARRANT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the invention is to provide a preparation method of high-purity docusate sodium, to solve the problem that the prior art cannot obtain docusate sodium with a purity higher than 99%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a 500mL three-necked flask equipped with a water separator, a reflux condenser and a thermometer, add 50g (0.5mol) of maleic anhydride, 230mL (1.50mol) of 2-ethylhexanol, and 1.0g of p-toluenesulfonic acid (5mmol), 50mL of toluene, shake well, heat the oil bath to reflux, control the internal temperature at 125-140°C, react for about 1.5hr, separate water 9mL from the water separator (theoretical amount of water generated is 9mL), stop the reaction, cool to light yellow The reaction solution was washed successively with an equal volume of water, 10% NaHCO 3 solution (100ml), and then washed with water (2 × 100mL), toluene and 2-ethylhexanol were recovered by distillation under reduced pressure to obtain 163.4g of di(2-ethyl)hexyl maleate in the form of light yellow oil, which was recovered from The rate is 96.0%.

[0024] Di(2-ethyl)hexyl maleate 340g (1.0mol), NaHSO 3 Add 125g (1.2mol) and 300mL of water into a 1000mL autoclave, seal it tightly, and stir and react...

Embodiment 2

[0027] The reaction operation steps are the same as in Example 1, and the purification steps are as follows: 410g of the crude product of docusate sodium is dissolved in 900mL of absolute ethanol, and there is a small amount of insoluble matter. Add 4 to 5g of activated carbon, filter, add 90mL of water and 90mL of toluene to the filtrate, After cooling to -5°C, crystals were precipitated, crystallized overnight, and filtered with suction to obtain 348 g of hydrous crystals. The crystals were dissolved in 1500 mL of absolute ethanol, and the ethanol was recovered under reduced pressure to obtain 314 g of powdered docusate sodium, with a sulfonation yield of 70.7% and a purity of 99.5%.

Embodiment 3

[0029]In a 1000mL three-necked flask equipped with a water separator, a reflux condenser and a thermometer, add 50g (0.5mol) of maleic anhydride, 230mL (1.50mol) of 2-ethylhexanol, and 25g of 001x7 (732) cation Exchange resin, 100mL of toluene, shake well, heat the oil bath to reflux, control the internal temperature at 100°C, react for about 3hrs, separate 9mL of water from the water separator (theoretical amount of water generated is 9mL), stop the reaction, cool the light yellow reaction solution, and filter The exchange resin was removed, the resin was washed twice with 50 mL of water, and toluene and 2-ethylhexanol were recovered by distillation under reduced pressure to obtain 163.4 g of di(2-ethyl)hexyl maleate in the form of light yellow oil, with a yield of 96.0%.

[0030] Di(2-ethyl)hexyl maleate 340g (1.0mol), NaHSO 3 Add 125g (1.2mol) and 300mL of water into a 1000mL autoclave, seal it tightly, and stir and react at 105-110°C for 8 hours to obtain a viscous, colorl...

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PUM

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Abstract

The invention relates to a method for preparing docusate sodium. The method comprises the step of esterification between 2-ethyl hexanol and maleic anhydride and the step of sulfonation of the obtained ester and sodium hydrogensulfite in a water solution. The method is characterized in that the method further comprises the following steps of purification of rough products: crystallizing the sulfonated rough products in an alcohol and water system to obtain a water-containing crystal, dissolving the water-containing crystal in alcohol dehydratum, performing reduced pressure distillation to remove a solvent so as to obtain anhydrous docusate sodium, wherein alcohol in the alcohol and water system is selected from a group comprising methyl alcohol, ethanol, normal propyl alcohol and isopropyl alcohol, and the alcohol dehydratum is selected from ethanol, normal propyl alcohol and isopropyl alcohol. By the method provided by the invention, the high-purity docusate sodium can be prepared.

Description

technical field [0001] The invention relates to a preparation method of organic matter, in particular to a preparation method of high-purity docusate sodium. Background technique [0002] Docusate Naocinate, also known as Dioctyl Sodium, Sulfosuceinate, is a surfactant. After oral administration, it can make water and fatty substances soak into the feces in the intestine to promote its softening. It is suitable for weak defecation such as anus, Proctopathy patients, or postoperative patients. The synthesis of docusate sodium usually adopts two-step method, the first step is to make maleic anhydride and 2-ethylhexanol carry out esterification reaction in the presence of mineral acid or organic acid; Sodium bisulfite undergoes sulfonation reaction in aqueous solution to obtain docusate sodium. Although docusate sodium has a large demand, the purity of the product supplied on the market is not high, about 95-96%. According to the literature disclosed in the prior art, the pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/17C07C303/44
Inventor 肖爱平周志刚肖利辉
Owner HUNAN WARRANT PHARMA
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