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Process for catalytically synthesizing isosorbierte by strong acid ion exchanging resin

A technology of ion exchange resin and isosorbide, applied in the direction of organic chemistry, isomerization preparation, etc., can solve the problems of shortening the service life of equipment, difficulty in handling after equipment cleaning, and generating waste residue environment, so as to achieve easy separation and elimination of reaction system Carbonization phenomenon, non-environmental pollution effect

Inactive Publication Date: 2003-06-25
QUFU NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Zhou Yuan, Shao Wei etc. have introduced the method that adopts sulfuric acid catalysis to prepare isosorbide in the preparation of isosorbide " Hubei Chemical Industry, 1999, (2) 11 ", and the weak point of sulfuric acid catalysis synthesis isosorbide is that this method It can cause corrosion to the equipment and shorten the service life of the equipment; cause serious carbonization, which makes it difficult to clean up the equipment and the post-processing of the product; the product yield is low; the catalyst is not easy to separate from the reaction system and reuse it many times
If it is used in industrial production, it will not only consume part of the raw materials due to carbonization, but also cause environmental pollution due to the generation of waste residues.

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0012] Example 1: In a 250-liter container equipped with a stirring device and a water separator, add 100 liters of 53% industrial sorbitol aqueous solution and 20 liters of toluene, start the agitator and heat to 115 ° C for dehydration, when the water is separated When there is no drop of water in the container, it indicates that the dehydration is over. Stop heating, then add 8 kg of strong acidic ion exchange resin catalyst, continue heating to 105 ° C for dehydration, react for about 5 hours, stop heating, add 30 liters of water to dilute, filter out strong acidic ion exchange resin and separate toluene, and then use distillation Remove a small amount of toluene, and when the distillation is about to end, use a vacuum pump to distill under reduced pressure, continue dehydration to obtain a crude product of isosorbide, and finally use an ethanol-ether mixture with an ethanol content of 3% to repeatedly crystallize to obtain a needle-shaped pure product of isosorbide 37 kg,...

Embodiment 2

[0013] Embodiment 2: in the container of 250 liters that agitator and water separator are housed, add 100 liters of 53% industrial sorbitol aqueous solution and 40 liters of toluene, start agitator and be heated to 100 ℃ for dehydration, when water separates When there is no drop of water in the container, it indicates that the dehydration is over. Stop heating, then add 14 kg of strong acidic ion exchange resin catalyst, continue heating to 110 ° C for dehydration, react for about 4 hours, stop heating, add 40 liters of water to dilute, filter out strong acidic ion exchange resin and separate toluene, and then use distillation Remove a small amount of toluene, and when the distillation is about to end, use a vacuum pump to distill under reduced pressure, continue dehydration to obtain a crude product of isosorbide, and finally use an ethanol-ether mixture with an ethanol content of 5% to repeatedly crystallize to obtain a needle-shaped pure product of isosorbide 37.3 kg, the ...

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Abstract

The synthesis process includes adding dewaternig agent solution in the amount of 10-50 wt% of industrial water solution of sorbierte to industrial water solution of sorbierte through stirring and heating to 100-120 deg.c to dewater sorbierte; adding strong acid ion exchanging resin as catalyst in the amount of 6-15 wt% of industrial water solution of sorbierte through stirring and heating to 104-110 deg.c to dewater until finishing the reaction; adding water to dilute and filtering out strong acid ion exchanging resin and separating dewatering agent; distilling to obtain course product; and re-crystallizing in mixed ethanol and ether solvent to obtain isosorbierte product.

Description

technical field [0001] The invention relates to the preparation of medicaments, more specifically to a method for synthesizing isosorbide. Background technique [0002] Isosorbide is an oral diuretic, which is mainly used clinically to treat hydrocephalus, increased intracranial pressure, and glaucoma caused by various diseases. It is also the intermediate for the synthesis of Span and Tween non-ionic surfactants and the raw material for the treatment of angina pectoris isosorbide nitrate. Zhou Yuan, Shao Wei etc. have introduced the method that adopts sulfuric acid catalysis to prepare isosorbide in the preparation of isosorbide " Hubei Chemical Industry, 1999, (2) 11 ", and the weak point of sulfuric acid catalysis synthesis isosorbide is that this method It can corrode the equipment and shorten the service life of the equipment; cause serious carbonization, which makes it difficult to clean up the equipment and post-treatment of the product; the product yield is low; the...

Claims

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Application Information

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IPC IPC(8): C07C29/56C07C33/02
Inventor 高根之赵斌孙玉希
Owner QUFU NORMAL UNIV
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