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Synthesis method for triiodo benzoic triformic acid

A synthesis method and technology of triformic acid, applied in the fields of oxidative preparation of carboxylic acid, organic chemistry, etc., can solve the problems of long reaction cycle and complicated reaction steps, and achieve the effect of short production cycle, good product purity, and single reaction process

Inactive Publication Date: 2014-02-26
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The disadvantages of this method are: First, the use of HNO in the nitrilation process 2 , KCN, CuCN will generate highly toxic hydrocyanic acid, and the reaction solution contains a large amount of copper ions
But the reaction steps are still relatively cumbersome and the reaction cycle is long

Method used

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  • Synthesis method for triiodo benzoic triformic acid
  • Synthesis method for triiodo benzoic triformic acid
  • Synthesis method for triiodo benzoic triformic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Embodiment 1: the synthetic method of triiodobenzenetricarboxylic acid, the steps are as follows:

[0031] Add 10g of triiodotrimethylbenzene, 120ml of pyridine, and 50ml of water into a 500ml four-necked flask equipped with a thermometer, a stirrer and a reflux condenser, stir and heat up to 60°C. A total of 100g of potassium manganate, the temperature naturally rose to 90°C, after the addition, the reaction temperature was kept at 85-95°C, reacted for 10h, suction filtered while it was hot, washed with 70ml of 5wt% potassium hydroxide solution, combined the filtrate and lotion After rotary evaporation until no pyridine remained, the solid was dissolved in 150 ml of water, the insoluble solid was removed by filtration, and the filtrate was adjusted to pH = 1 with 36.5 wt% concentrated hydrochloric acid. Stir and acidify for 15 minutes, extract five times with 250ml of ethyl acetate, wash the combined extracts with 20ml of water, and rotary evaporate the oil phase to dr...

Embodiment 2

[0032] Embodiment 2: the synthetic method of triiodobenzenetricarboxylic acid, the steps are as follows:

[0033] Add 10g of triiodotrimethylbenzene, 120ml of pyridine, and 50ml of water into a 500ml four-necked flask equipped with a thermometer, a stirrer and a reflux condenser, stir and heat up to 60°C, once an hour, add 20g each time in 4 batches A total of 80g of potassium manganate, the temperature naturally rose to 90°C, after the addition, the reaction temperature was kept at 85-95°C, reacted for 10h, filtered while hot, washed with 70ml of 5wt% potassium hydroxide solution, combined the filtrate and washing liquid Rotary evaporate until no pyridine remains, dissolve the solid in 150ml of water, remove the insoluble solid by filtration, and adjust the pH of the filtrate to 1 with 36.5wt% hydrochloric acid. Stir and acidify for 15 minutes, extract five times with 250ml of ethyl acetate, wash the combined extracts with 15ml of water, and rotary evaporate the oil phase to ...

Embodiment 3

[0034] Embodiment 3: the synthetic method of triiodobenzenetricarboxylic acid, the steps are as follows:

[0035] Add 10g of triiodotrimethylbenzene, 120ml of pyridine, and 50ml of water into a 500ml four-necked flask equipped with a thermometer, a stirrer and a reflux condenser, stir and heat up to 60°C, once an hour, add 20g each time in 6 batches A total of 120g of potassium manganate, the temperature naturally rose to 90 ° C, the reaction temperature was kept at 85-95 ° C after the addition, reacted for 10 hours, suction filtered while it was hot, washed with 70 ml of 5wt% potassium hydroxide solution, and the filtrate and washing liquid were combined Rotary evaporate until no pyridine remains, dissolve the solid in 150ml of water, remove the insoluble solid by filtration, and adjust the pH of the filtrate to 1 with 36.5wt% hydrochloric acid. Stir and acidify for 15 minutes, extract five times with 250ml ethyl acetate, wash the combined extracts with 20ml water, and rotary...

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Abstract

The invention relates to a synthesis method for a triiodo benzoic triformic acid, which comprises the following steps: generating the triiodo benzoic triformic acid by utilizing the single-step oxidation of potassium permanganate by taking triiodo trimethylbenzene as a starting raw material and directly taking mixed liquor of water and pyridine as a solvent at the temperature of 85-95 DEG C; then, performing vacuum rotary evaporation to remove the water and the pyridine; and performing acidification, ethyl acetate extraction and drying by distillation on a solid to obtain the triiodo benzoic triformic acid. The synthesis method has the advantages that the reaction raw material does not have strong corrosion on equipment; the reaction process is single; the operation is simple; the production cycle is short; the equipment investment is low; the reaction speed is high; the yield is high and the like.

Description

technical field [0001] The invention relates to a synthesis method of triiodobenzenetricarboxylic acid, which belongs to the field of chemical synthesis. technical background [0002] Triiodobenzenetricarboxylic acid is an important intermediate in the synthesis of triiodobenzenetricarboxamide, a non-ionic fluoroscopy contrast agent. These compounds have aroused great interest due to their good pharmacological properties. However, due to the difficulty in synthesis, no commercially valuable compound has been obtained so far. The discovery of triiodobenzenetricarboxylic acid has reflected the excellent performance of this compound, and has the possibility of further development with its low cost. [0003] According to existing bibliographical reports, the synthesis of triiodobenzenetricarboxylic acid mainly contains the following methods: [0004] 1. Using nitroisophthalic acid as raw material, first reduce the nitro group to amino group, then iodide with iodine chloride, t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C63/68C07C51/16
Inventor 杨延钊盛道鹏
Owner SHANDONG UNIV