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Method for preparing high-purity docusate sodium

A docusate sodium, high-purity technology, applied in the field of preparation of high-purity docusate sodium, can solve the problems of low yield, cumbersome process, and long time consumption

Inactive Publication Date: 2015-08-12
BEIJING BANGNIKANGDA MEDICAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The market demand of docusate sodium is very large, but there are almost no high-purity products, and there are few reports on the method for preparing high-purity docusate sodium. method of the product
However, this method still has the disadvantages of low yield, cumbersome process, long time consumption, and the use of toxic reagents such as toluene.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1. Esterification of maleic anhydride and isooctyl alcohol

[0037] In a 3L three-necked flask, 392g of maleic anhydride, 936g of isooctyl alcohol and 7.6g of p-toluenesulfonic acid were added under nitrogen protection. First, stir and react at 90°C under normal pressure for 10 minutes. When there is no maleic anhydride solid in the reaction system, raise the temperature to 120°C and heat to reflux, and use an oil-water separator under the condition of water pump decompression (5.33KPa) The water formed by the reaction was removed. After reacting for 3 hours, stop heating, cool to room temperature and wash with saturated Na 2 CO 3 The solution was washed twice, the aqueous phase was discarded, and the organic phase was washed three times with deionized water. Anhydrous Mg was added to the organic phase 2 SO 4 Dry, filter, and use an oil pump to distill under reduced pressure (0.4KPa), collect fractions at 130°C to obtain 1118g of a colorless and transparent diisooc...

Embodiment 2

[0043] 1. Esterification of maleic anhydride and isooctyl alcohol

[0044] In a 3L three-necked flask, 392g of maleic anhydride, 990g of isooctyl alcohol and 3.8g of p-toluenesulfonic acid were added under nitrogen protection. First, stir and react at 85°C under normal pressure for 15 minutes. When there is no maleic anhydride solid in the reaction system, raise the temperature to 115°C and heat to reflux, and use an oil-water separator under the condition of water pump decompression (4.33KPa) The water formed by the reaction was removed. After reacting for 2 hours, stop heating, cool to room temperature and wash with saturated Na 2 CO 3 The solution was washed twice, the aqueous phase was discarded, and the organic phase was washed three times with deionized water. Anhydrous Mg was added to the organic phase 2 SO 4 Dry, filter, and use an oil pump to distill under reduced pressure (0.3KPa), collect fractions at 130°C to obtain 1198g of a colorless and transparent diisooc...

Embodiment 3

[0048] 1. Esterification of maleic anhydride and isooctyl alcohol

[0049] In a 3L three-necked flask, 392g of maleic anhydride, 936g of isooctyl alcohol and 11.4g of p-toluenesulfonic acid were added under nitrogen protection. First, stir and react at 95°C under normal pressure for 10 minutes. When there is no maleic anhydride solid in the reaction system, raise the temperature to 125°C and heat to reflux, and use an oil-water separator under the condition of water pump decompression (6.33KPa) The water formed by the reaction was removed. After reacting for 3 hours, stop heating, cool to room temperature and wash with saturated Na 2 CO 3 The solution was washed 3 times, the aqueous phase was discarded, and the organic phase was washed 2 times with deionized water. Anhydrous Mg was added to the organic phase 2 SO 4 Dry, filter, and use an oil pump to distill under reduced pressure (0.4KPa), collect the fraction at 130°C to obtain 1112g of a colorless and transparent diiso...

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Abstract

The invention provides a method for preparing high-purity docusate sodium. The method includes esterification of maleic anhydride and isooctanol and sulfonation of obtained diesters and sodium hydrogen sulfite in aqueous solution; wherein the esterification and sulfonation are completed under nitrogen protection, and the esterification is divided into 80-95 DEG C pre-esterification and 115-125 DEG C decompression reaction. By the method simple in process, little in toxic solvent, free of pollution and high in yield, the prepared docusate sodium is high in purity.

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 sulfosuccinate sodium salt, is a class of anionic surfactants with excellent penetration and wetting properties, and has been widely used in textiles, printing and dyeing, coatings, In the fields of papermaking, medicine, pesticide, daily chemical industry, etc., after oral administration, water and fatty substances can be soaked into the feces in the intestine to promote softening. It is suitable for patients with inability to defecate, such as anal and rectal diseases, or postoperative patients. The synthesis of docusate sodium usually adopts two-step method, the first step is to make maleic anhydride and isooctyl alcohol carry out esterification reaction under the catalysis of mineral acid or organic acid; Sodium bisulfate undergoes sulfonation rea...

Claims

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Application Information

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IPC IPC(8): C07C309/17C07C303/32B01J31/02
Inventor 薛志勇张昊江峰张梅玲
Owner BEIJING BANGNIKANGDA MEDICAL TECH CO LTD
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