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A kind of preparation method of 5-amino-2,4,6-triiodoisophthalic acid

A technology of triiodoisophthalic acid and aminoisophthalic acid, which is applied in the field of preparation of 5-amino-2,4,6-triiodoisophthalic acid, can solve difficult operation, many solid wastes and instability and other problems, to achieve the effect of reducing the pressure of water treatment, less solid waste and ideal yield

Active Publication Date: 2022-04-29
江苏丽源医药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of these methods require the use of highly toxic, unstable and difficult-to-handle oxidants or iodinated reagents, and there are many solid wastes

Method used

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  • A kind of preparation method of 5-amino-2,4,6-triiodoisophthalic acid

Examples

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Embodiment 1

[0022] This example provides a preparation method of 5-amino-2,4,6-triiodoisophthalic acid, the reaction route and principle are as follows:

[0023]

[0024] The preparation method of described 5-amino-2,4,6-triiodoisophthalic acid comprises the steps:

[0025] Add 10mmol 5-aminoisophthalic acid (1.79g), 60mmol KI (9.96g), 60mmol DMSO (3.12g), 90mmol HCl (7.5mL concentrated hydrochloric acid (mass fraction of hydrogen chloride is about 37%)) to 3000mmol water (54 mL), stirred at room temperature for 10 min. The temperature was raised to 100°C to continue the reaction for 16h. After the reaction was completed, it was lowered to room temperature, filtered, and the obtained solid was dissolved in 1M KOH (30 mL), and treated with activated carbon for decolorization. Then add 1M HCl to neutralize to acidity, filter, pickle (1M HCl 10mL×3), and dry to obtain the final solid product 5-amino-2,4,6-triiodoisophthalic acid with a yield of 70%. 95% purity.

Embodiment 2

[0027] This example provides a kind of preparation method of 5-amino-2,4,6-triiodoisophthalic acid, described preparation method comprises the following steps: 10mmol 5-aminoisophthalic acid (1.79g), 60mmol NaI ( 9g), 60mmol DMSO (3.12g), 90mmol HCl (7.5mL concentrated hydrochloric acid) were added to 3000mmol water (54mL), and stirred at room temperature for 10min. The temperature was raised to reflux to continue the reaction for 16h. After the reaction was completed, it was lowered to room temperature, filtered, and the resulting solid was dissolved in 1M KOH (30 mL), and treated with activated carbon for decolorization. Then add 1M HCl to neutralize to acidity, filter, pickle (1M HCl 10mL×3), and dry to obtain the final solid product 5-amino-2,4,6-triiodoisophthalic acid with a yield of 68%. 91% purity.

Embodiment 3

[0029] This example provides a preparation method of 5-amino-2,4,6-triiodoisophthalic acid, the preparation method comprising the following steps: 10mmol 5-aminoisophthalic acid (1.79g), 60mmol NH 4 I (8.7g), 60mmol DMSO (3.12g), 90mmol HCl (7.5mL concentrated hydrochloric acid) were added to 3000mmol water (54mL), and stirred at room temperature for 10min. The temperature was raised to reflux to continue the reaction for 16h. After the reaction was completed, it was lowered to room temperature, filtered, and the resulting solid was dissolved in 1M KOH (30 mL), and treated with activated carbon for decolorization. Then add 1M HCl to neutralize to acidity, filter, pickle (1M HCl 10mL×3), and dry to obtain the final solid product 5-amino-2,4,6-triiodoisophthalic acid with a yield of 73%. 90% purity.

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Abstract

The invention discloses a preparation method of 5-amino-2,4,6-triiodoisophthalic acid. The preparation method comprises the following steps: making 5-aminoisophthalic acid, iodine salt and Dimethyl sulfoxide reacts in a solvent to generate 5-amino-2,4,6-triiodoisophthalic acid; wherein, the solvent is water and / or C1-6 alcohol solvent; this method not only abandons existing There are highly toxic, unstable and difficult-to-operate oxidizing agents or iodine reagents that are often used in the technology, and the whole synthesis process has less solid waste, which reduces the pressure of water treatment, and the yield is also relatively ideal.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of 5-amino-2,4,6-triiodoisophthalic acid. Background technique [0002] 5-Amino-2,4,6-triiodoisophthalic acid is the main raw material of many X-ray contrast agents (Organic & Biomolecular Chemistry, 2006, 4, 3611; Tetrahedron Letters, 2002, 43, 561). [0003] The method for synthesizing this compound is mainly following several at present: (1) ICl reacts with KCl to generate KICl 2 , which is used as an iodination reagent to synthesize 5-amino-2,4,6-triiodoisophthalic acid (Organic & Biomolecular Chemistry, 2006, 4, 3611) by electrophilic iodination reaction; (2) KI reacts with chlorine to generate KICl 2 , which reacts with 5-aminoisophthalic acid to generate the target product (Tetrahedron Letters, 2002,43,561); (3) KI and oxides (such as KIO 3 ) reaction in situ to form electrophilic iodine species, and react with 5-aminoisophthalic acid to ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C229/60C07C227/16
CPCC07C227/16C07C229/60
Inventor 杨盟孙璐马圣峰顾晓春
Owner 江苏丽源医药有限公司
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