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Method for purifying ioversol

A purification method, the technology of ioversol, which is applied in the separation/purification of carboxylic acid amide, organic chemistry, etc., can solve the problems that ioversol cannot be completely purified

Inactive Publication Date: 2005-04-20
JIANGSU INST OF NUCLEAR MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can only remove impurities with a molecular weight below 400, and the molecular weight of non-ionic impurities is close to the molecular weight of ioversol 807, so this method cannot completely purify ioversol, and can only remove some small molecular weight impurities

Method used

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  • Method for purifying ioversol

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Experimental program
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Effect test

Embodiment 1

[0022] In a 3L three-necked flask equipped with an electric stirrer and a reflux condenser, the crude ioversol (45g) was added to n-butanol (2250mL), and the temperature was gradually raised to reflux under stirring, and refluxed for 5 hours, then filtered the white The suspension was washed with hot n-butanol (3×15 mL) on the filter and dried in vacuo to obtain 27.5 g of ioversol. HPLC analysis (water / acetonitrile, C 8 column). The results are shown in Table 1.

[0023] Dissolve ioversol (27.5g) obtained in the first recrystallization above in water (150mL), evaporate to dryness under reduced pressure and add n-butanol (1375mL) to carry out the second recrystallization, the operation steps are the same as the first recrystallization Crystallization, to get ioversol 19.3g, carry out HPLC analysis (water / acetonitrile, C 8 column). The results are shown in Table 1.

[0024] the peak

Embodiment 2

[0026] In a 1L three-neck flask equipped with an electric stirrer and a reflux condenser, the ioversol crude product (45g) was added to a mixture of 2-methoxyethanol (135mL) and isopropanol (540mL), and the temperature was gradually raised to Keep the temperature at 100°C for 5 hours, then filter the white suspension while hot, wash the crystals with hot isopropanol (3×15 mL) on the filter, and dry in vacuo to obtain 29.2 g of ioversol. HPLC analysis (water / acetonitrile, C 8 column). The results are shown in Table 2.

[0027] Dissolve ioversol (29.2g) obtained in the first recrystallization above in water (150mL), evaporate to dryness under reduced pressure, add 2-methoxyethanol (88mL) and isopropanol (350mL), and carry out the second Recrystallization, operation steps are the same as first time recrystallization, get ioversol 20.8g, carry out HPLC analysis (water / acetonitrile, C 8 column). The results are shown in Table 2.

[0028] the peak

Embodiment 3

[0030] In a 1L three-necked flask equipped with an electric stirrer and a reflux condenser, add crude ioversol (45 g) into a mixture of 2-methoxyethanol (90 mL) and n-butanol (600 mL), and gradually heat up to 100 °C under stirring. ℃, keep the temperature constant for 5 hours, then filter the white suspension while hot, wash the crystals with hot n-butanol (3×15 mL) on the filter, and dry in vacuo to obtain 31.5 g of ioversol. HPLC analysis (water / acetonitrile, C 8 column). The results are shown in Table 3.

[0031] Dissolve ioversol (31.5g) obtained in the first recrystallization above in water (150mL), evaporate to dryness under reduced pressure, add 2-methoxyethanol (63mL) and n-butanol (420mL), carry out the second recrystallization Crystallization, the operating steps are the same as the first recrystallization, to get ioversol 25g, carry out HPLC analysis (water / acetonitrile, C 8 column). The results are shown in Table 3.

[0032] the peak

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Abstract

A method for purifying ioversol, the invention relates to a method for purifying ioversol as an x-ray non-ionic contrast agent. The method adopts the solvent recrystallization method to carry out two recrystallizations to the ioversol crude product, and the recrystallization solvent used includes: n-butanol, 2-methoxyethanol and isopropanol mixed solvent, 2-methoxyethanol and n-butanol Solvents are mixed, and the content of ioversol reaches more than 99.0% after recrystallization. The method is economical and practical, easy to operate and suitable for industrial production.

Description

technical field [0001] The invention belongs to a purification method of western medicine compounds, in particular to a purification method of ioversol, an X-ray non-ionic contrast agent. Background technique [0002] In 1982, U.S. Wanlingke Company successfully developed the non-ionic contrast agent Ioversol (Ioversol, the trade name is Ansheli, Optiray), and the chemical name is N, N'-bis(2,3-dihydroxypropyl) -5-[N-(2-hydroxyethyl)-glycolamide]-2,4,6-triiodo-1,3-benzenedicarboxamide, see structural formula 1 for the chemical structure. [0003] Structural formula one: [0004] [0005] Ioversol water solubility is very good, and osmotic pressure is also very low, and chemical property is also more stable, can withstand high temperature sterilization, can be made into injection supply market, can be widely used in blood vessel (applicable to angiography, urinary tract contrast, venography, and contrast-enhanced computer scan), subarachnoid applications (for lumbar, tho...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/24C07C237/46
Inventor 邹霈罗世能刘娅灵谢敏浩何拥军
Owner JIANGSU INST OF NUCLEAR MEDICINE
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