Method for preparing 5-amino-N,N'-di(2,3-dihydroxypropyl)-2,4,6-triiodoisophthal amide

A technology of triiodoisophthalamide and dihydroxypropyl, which is used in the preparation of 5-amino-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide In the field of preparation, it can solve problems such as high production costs, dangerous operators, and complex preparation processes, and achieve the effects of reducing environmental impact, production costs, and equipment corrosion.

Inactive Publication Date: 2012-04-04
JIANGSU INST OF NUCLEAR MEDICINE
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0003] The third-generation non-ionic contrast agent has many reaction steps, complicated preparation process, and high production cost, resulting in expensive clinical use
Iodine monochloride is a poisonous, harmful and highly corrosive product. It has strict requirements on packaging, transportation and use. Improper use will cause danger to operators, and the yield of the original preparation method is not high, and the production cost is very high. Therefore, it is necessary to The preparation method of 5-amino-N, N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide is improved, and a process with mild reaction conditions, easy operation, and less corrosion to equipment is designed. The reaction yield is high, and the production process suitable for industrial production

Method used

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  • Method for preparing 5-amino-N,N'-di(2,3-dihydroxypropyl)-2,4,6-triiodoisophthal amide

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Add 16.5 grams of potassium iodide and 1M hydrochloric acid to the 5-amino-N, N'-bis(2,3-dihydroxypropyl) isophthalamide solution obtained in the reduction reaction to adjust the pH to 1-2, and add 4.4 grams of sodium chlorite , stirred and reacted at 0°C for 1 hour, adjusted the pH of the solution to neutral with 1M NaOH, left the filtrate at room temperature to precipitate a solid, filtered, and dried at 70°C to obtain 18.2 g, with a yield of 51.7%.

Embodiment 2

[0021] Add 33.1 grams of potassium iodide and 1M hydrochloric acid to the 5-amino-N, N'-bis(2,3-dihydroxypropyl)isophthalamide solution obtained in the reduction reaction to adjust the pH to 1-2, and add 17.8 grams of sodium chlorite , stirred and reacted at 50°C for 8 hours, adjusted the pH of the solution to neutral with 1M NaOH, left the filtrate at room temperature to precipitate solids, filtered, and dried at 70°C to obtain 21.2 g, with a yield of 60.3%.

Embodiment 3

[0023] Add 21.4

[0024] Adjust the pH to 1-2 with 1 g of potassium iodide and 1M hydrochloric acid, add 5.3 g of sodium chlorite, stir and react at 15°C for 3 hours, adjust the pH of the solution to neutral with 1M NaOH, leave the filtrate at room temperature to precipitate solids, filter, and dry at 70°C , to obtain 25.5 grams, yield 72.5%.

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Abstract

The invention discloses a method for preparing 5-amino-N,N'-di(2,3-dihydroxypropyl)-2,4,6-triiodoisophthal amide, and belongs to the technical field of pharmaceutical intermediates. The compound is an important intermediate of non-ionic x-ray contrast agents of iohexol and ioversol. The invention provides process reaction conditions for preparing the 5-amino-N,N'-di(2,3-dihydroxypropyl)-2,4,6-triiodoisophthal amide; and the process reaction conditions are mild, the operation is simple and convenient, corrosion to equipment is low, the reaction yield is high, the production cost is obviously reduced, and the industrial production of the product is easy to implement.

Description

technical field [0001] A preparation method of 5-amino-N, N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide, involving 5-nitro-N, N'- Bis(2,3-dihydroxypropyl)isophthalamide is used as raw material, and 5-amino-N,N'-bis(2,3-dihydroxypropyl)isophthalamide is obtained by reduction reaction, and then iodination Reaction, using potassium iodide as the iodine source, sodium chlorite as the oxidant, and preparing 5-amino-N, N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo through iodination reaction Isophthalamide. 5-Amino-N, N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide is an important pharmaceutical intermediate, mainly used in non-ionic X-ray contrast The preparation of iohexol (Iohexol) and ioversol (Ioversol). Background technique [0002] Contrast media (also known as contrast media, contrast media) is one of the most commonly used drugs in interventional radiology operations. It is mainly used for the display of blood vessels and body cavities. There are various ...

Claims

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Application Information

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IPC IPC(8): C07C237/46C07C231/12
Inventor 谢敏浩王洪勇吴昊邹霈刘娅灵何拥军
Owner JIANGSU INST OF NUCLEAR MEDICINE
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