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Synthetic method of ioversol

A synthetic method, the technology of ioversol, which is applied in the field of organic compound preparation, can solve the problems of complex process, difficult synthesis of ioversol, low quality and yield, etc., to simplify the synthesis process, improve quality and yield, and reduce desalination The effect of the craft

Inactive Publication Date: 2019-01-29
HUBEI TIANSHU PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The quality and yield of traditional ioversol products in the synthesis preparation are low, and salts will be generated during the synthesis, which will affect the purity of ioversol during the recrystallization process of ioversol. Desalination, but the process is more complicated, and it is not easy to synthesize ioversol. Therefore, we propose a synthetic method for ioversol

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The present invention proposes a kind of synthetic method of ioversol, comprises the following steps:

[0015] S1. First, the ioversol intermediate 5-chloroacetamido-N, N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzenedicarboxamide Dissolved in a mixed solution of methanol, ethanol and barium hydroxide, stirred thoroughly and raised the temperature to 40 degrees Celsius, then added 2-chloroethanol to carry out nitrogen alkylation reaction for 9 hours to generate the target product ioversol;

[0016] S2. The mixed solution obtained in S1 is subjected to depressurization distillation, methanol is separated first, and the barium chloride generated after the nitrogen alkylation reaction is dissolved in methanol and insoluble in ethanol, and the barium chloride is separated by precipitation and filtration;

[0017] S3. After completing S2, the solution containing the target product ioversol is recrystallized with propylene glycol monomethyl ether, the temperature is cont...

Embodiment 2

[0020] The present invention proposes a kind of synthetic method of ioversol, comprises the following steps:

[0021] S1. First, the ioversol intermediate 5-chloroacetamido-N, N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzenedicarboxamide Dissolved in a mixed solution of methanol, ethanol and barium hydroxide, stirred thoroughly and raised the temperature to 50 degrees Celsius, then added 2-chloroethanol for nitrogen alkylation reaction for 10 hours to generate the target product ioversol;

[0022] S2. The mixed solution obtained in S1 is subjected to depressurization distillation, methanol is separated first, and the barium chloride generated after the nitrogen alkylation reaction is dissolved in methanol and insoluble in ethanol, and the barium chloride is separated by precipitation and filtration;

[0023] S3, after completing S2, recrystallize the solution containing the target product ioversol with propylene glycol monomethyl ether, control the temperature at 100 degr...

Embodiment 3

[0026] The present invention proposes a kind of synthetic method of ioversol, comprises the following steps:

[0027] S1. First, the ioversol intermediate 5-chloroacetamido-N, N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzenedicarboxamide Dissolved in a mixed solution of methanol, ethanol and barium hydroxide, stirred thoroughly and raised the temperature to 50 degrees Celsius, then added 2-chloroethanol for nitrogen alkylation reaction for 11 hours to generate the target product ioversol;

[0028] S2. The mixed solution obtained in S1 is subjected to depressurization distillation, methanol is separated first, and the barium chloride generated after the nitrogen alkylation reaction is dissolved in methanol and insoluble in ethanol, and the barium chloride is separated by precipitation and filtration;

[0029] S3. After completing S2, the solution containing the target product ioversol is recrystallized with propylene glycol monomethyl ether, the temperature is controlled a...

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PUM

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Abstract

The invention discloses a synthetic method of ioversol. The synthetic method comprises the following steps: firstly, dissolving an ioversol intermediate 5-chloroacetamido-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzenedicarboxamide into a mixed solution of methanol, ethanol and barium hydroxide, and then adding 2-chloroethanol to carry out a nitrogen alkylation reaction to obtain a targetproduct ioversol; carrying out reduced pressure distillation on the obtained mixed solution to separate out the methanol, and separating out barium chloride by precipitation filtration according to the fact that the barium chloride generated after the nitrogen alkylation reaction is soluble in methanol and is insoluble in ethanol; and finally recrystallizing the solution containing the target product ioversol by using propylene glycol monomethyl ether to obtain the target product ioversol. According to the synthetic method disclosed by the invention, the quality and the yield of the synthesisof the ioversol are effectively improved, and the synthesis process is simplified.

Description

technical field [0001] The invention relates to the technical field of organic compound preparation, in particular to a synthetic method of ioversol. Background technique [0002] Ioversol is mainly used in various vascular radiographic examinations, including: cerebral angiography, peripheral arteriography, visceral artery, renal artery and aorta angiography, and cardiovascular angiography including coronary angiography, arterial and venous digital subtraction angiography Angiography, etc. Intravenous urography and enhanced CT examination (including head and body CT), etc. The quality and yield of traditional ioversol products in the synthesis preparation are low, and salts will be generated during the synthesis, which will affect the purity of ioversol during the recrystallization process of ioversol. desalination, but the process is relatively complicated, and it is not easy to synthesize ioversol. Therefore, we have proposed a synthetic method for ioversol. Contents ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C237/46C07C231/12C07C231/24
CPCC07C231/12C07C231/24C07C237/46
Inventor 刘云龙
Owner HUBEI TIANSHU PHARMA CO LTD
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