Process for purifying ioversol

A technology for ioversol and ethanol, applied in the field of purifying ioversol, can solve the problems of large amount of solvent consumption, troublesome water-soluble evaporation and low final yield, etc., and achieves improving product yield, shortening refining cycle, and controlling production cost effect

Active Publication Date: 2009-01-07
JIANGSU HENGRUI MEDICINE CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method consumes a large amount of solvent, and it is troublesome to dissolve and evaporate to dryness. The final yield is low, and the requirements for moisture control are relatively high. , refinement failed

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 10g of crude ioverol (purity 92.9%, moisture 1.13%) to the reaction flask, add 200 mL of absolute ethanol, and heat to reflux with rapid stirring. The reaction solution is gradually clarified. After the solution is clear, the ethanol is evaporated at atmospheric pressure. When the ethanol is evaporated Add a little seed crystal at 80mL to start crystallization, reflux and stir for 2h, cool to 50℃ and then stir for 3h, precipitate more crystals, filter while hot, wash twice with a small amount of ethanol, drain and dry to obtain iodine The primary alcohol refined product is 8.1 g, with a purity of 98.1% and a yield of 81.0%.

[0016] Ioverol primary refined product (purity 98.1%, moisture 1.47%), 8.0g, was added to the reaction flask, 120mL ethanol was added, and heated to reflux with rapid stirring. The reaction solution was gradually clarified. After the solution was clear, the ethanol was evaporated at atmospheric pressure. Add a little seed crystals when 24mL of etha...

Embodiment 2

[0018] Add 10g of crude ioverol (purity 92.9%, moisture 1.56%) into the reaction flask, add 200 mL of ethanol, and heat to reflux with rapid stirring. The reaction solution is gradually clarified. After the solution is clear, the ethanol is evaporated. When 60 mL of ethanol is evaporated, Add seed crystals, and the seed crystals will dissolve immediately until 80mL is evaporated. Add the seed crystals and start crystallization. After refluxing for 2 hours, cool to 50°C and stir for 3 hours. More solids are precipitated. Filter while hot. Wash twice with a small amount of ethanol. After drying and drying, 8.6 g of refined ioverol is obtained with a purity of 98.5% and a yield of 86.0%.

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Abstract

The invention relates to a method for purifying ioversol that is x-ray nonionic contrast agent. The method adopts ethanol as recrystallization solvent to recrystallize ioversol crude-product, and the content of the obtained ioversol pure-product is more than 98.5 percent. The method is simple, easy to operate, economical and practical, and suitable for large-scale industrial production.

Description

Technical field [0001] The present invention relates to a method for purifying ioverol, which is widely used as an X-ray non-ionic contrast agent. Background technique [0002] So far, ioverol is widely used as a safe X-ray non-ionic contrast agent, and it has the characteristics of good water solubility, low osmotic pressure, and relatively stable chemical properties. It is an ideal contrast agent widely used in angiography. Venography, arthrography, urography, chest and cervical spine angiography, gastrointestinal examination, etc. However, ioverol, as a vascular injection, requires relatively high purity. Therefore, it is necessary to study an effective method of purifying ioverol. [0003] The crude ioverol contains some non-ionic impurities, mainly 5-amino-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzenedi Formamide; 5-[[N-(2-hydroxyethyl)carbamoyl]methoxy]-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo -1,3-phthalamide; 5-hydroxyacetamido-N,N'-bis(2,3-dihydroxypropyl)-2...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C237/46C07C231/24A61K49/04
Inventor 孙飘扬谭友建陈永江
Owner JIANGSU HENGRUI MEDICINE CO LTD
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