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Method for purifying ioversol

A purification method and technology of ioversol, applied in the separation/purification of carboxylic acid amides, organic chemistry and other directions, can solve the problems such as the inability to purify ioversol completely

Inactive Publication Date: 2004-03-24
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
  • Method for purifying ioversol

Examples

Experimental program
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Effect test

Embodiment 1

[0021] In a 3L three-necked flask equipped with an electric stirrer and reflux condenser, add the crude ioverol (45g) to n-butanol (2250mL), gradually increase the temperature to reflux with stirring, reflux for 5 hours, and then filter the white while hot The suspension was washed with hot n-butanol (3×15 mL) on the filter and the crystals were dried in vacuum to obtain 27.5 g of ioverol. HPLC analysis (water / acetonitrile, C 8 column). The results are shown in Table 1.

[0022] Dissolve ioverol (27.5g) obtained from the first recrystallization above in water (150mL), evaporate to dryness under reduced pressure, add n-butanol (1375mL), carry out the second recrystallization, the operation steps are the same as the first recrystallization Crystallized to obtain 19.3 g of ioverol, which was analyzed by HPLC (water / acetonitrile, C 8 column). The results are shown in Table 1.

[0023] Peak

Embodiment 2

[0025] In a 1L three-necked flask equipped with an electric stirrer and a reflux condenser, add the crude ioverol (45g) to the mixture of 2-methoxyethanol (135mL) and isopropanol (540mL), and gradually raise the temperature to Keep the temperature constant 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 ioverol. HPLC analysis (water / acetonitrile, C 8 column). The results are shown in Table 2.

[0026] Dissolve ioverol (29.2g) obtained from the first recrystallization in water (150mL), evaporate to dryness under reduced pressure, add 2-methoxyethanol (88mL) and isopropanol (350mL) for the second time Recrystallization, the procedure is the same as the first recrystallization, 20.8g of ioverol was obtained, which was analyzed by HPLC (water / acetonitrile, C 8 column). The results are shown in Table 2.

[0027] Peak

Embodiment 3

[0029] In a 1L three-necked flask equipped with an electric stirrer and a reflux condenser, add the crude ioverol (45g) to the mixture of 2-methoxyethanol (90mL) and n-butanol (600mL), and gradually increase the temperature to 100 with 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 vacuum to obtain 31.5 g of ioverol. HPLC analysis (water / acetonitrile, C 8 column). The results are shown in Table 3.

[0030] Dissolve ioverol (31.5g) obtained from the first recrystallization in water (150mL), evaporate to dryness under reduced pressure, add 2-methoxyethanol (63mL) and n-butanol (420mL) for the second recrystallization Crystallization, the operation steps are the same as the first recrystallization, and 25g ioverol is obtained, and analyzed by HPLC (water / acetonitrile, 8 column). The results are shown in Table 3.

[0031] Peak

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Abstract

The present invention relates to a purification method of X-ray non-ionic contrast agent ioversol. Said invention adopts the solvent recrystallization method to make the ioversol crude product undergo the process of recrystallization at twice, and its used recrystallization solvent includes: normal butyl alcohol, 2-methyl cellosolve and isopropanol mixed solvent and 2-methyl cellosolve and normal butyl alcohol mixed solvent. After having being recrystallized the content of the ioversol can be up to above 99.0%.

Description

Technical field [0001] The invention belongs to a method for purifying western medicine compounds, and specifically relates to a method for purifying ioversol, an X-ray non-ionic contrast agent. Background technique [0002] In 1982, the United States Vanlink Corporation successfully developed a non-ionic contrast agent Ioversol (Ioversol, trade name Optiray), with a chemical name of N,N′-bis(2,3-dihydroxypropyl) -5-[N-(2-hydroxyethyl)-hydroxyacetamido]-2,4,6-triiodo-1,3-phthalamide, the chemical structure is shown in structural formula 1. [0003] Structural formula one: [0004] [0005] Ioverol has good water solubility, low osmotic pressure, stable chemical properties, and can withstand high temperature sterilization. It can be made into injections for the market and can be widely used in blood vessels (applicable to angiography, urinary tract Angiography, venography and contrast-enhanced computer scanning), subarachnoid applications (for adults and children's lumbar, thora...

Claims

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Application Information

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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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