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Method for preparing high-purity docusate sodium

A docusate sodium and esterification technology, which is applied in the field of preparation of high-purity docusate sodium, can solve the problems of inability to obtain purity and high docusate sodium

Active Publication Date: 2014-01-22
HUNAN WARRANT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of this invention is to provide a kind of preparation method of high-purity docusate sodium, to solve the problem that prior art can not obtain the docusate sodium with 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 as light yellow oil, which was collected 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 at 105-110°C for 8...

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, and 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-neck 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 25g001x7 (732) cation exchange Resin and toluene 100mL, shake well, heat the oil bath to reflux, control the internal temperature at 100°C, react for about 3hr, separate out 9mL of water in the water separator (theoretical water volume is 9mL), stop the reaction, cool the light yellow reaction liquid, filter to remove The resin was exchanged, the resin was washed twice with 50 mL of water, the toluene and 2-ethylhexanol were recovered by distillation under reduced pressure, and 163.4 g of di(2-ethyl)hexyl maleate was obtained as 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, colorless and transparent liqui...

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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 sodium, also known as Dioctyl Sodium, Sulfosuceinate, is a surfactant. After oral administration, it can soak water and fatty substances into the feces in the intestines to promote their 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 relatively 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, t...

Claims

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Application Information

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Patent Type & Authority Patents(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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