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Preparation method of 2,4,6-triiodoresorcinol

A technology for triiodoresorcinol and resorcinol, which is applied in the field of preparation of iodophenol, can solve the problems of adding strong base yield, complex synthesis process route, etc., and achieves green reaction, process safety and controllability, and yield high effect

Active Publication Date: 2018-10-16
SINOPHARM CHEM REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0018] The object of the present invention is to provide a kind of preparation method of 2,4,6-triiodoresorcinol, to solve the complex process route of 2,4,6-triiodoresorcinol in the prior art, need to add Problems with strong base or low yield, etc.

Method used

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  • Preparation method of 2,4,6-triiodoresorcinol

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Experimental program
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Effect test

Embodiment 1

[0037] A kind of preparation method of 2,4,6-triiodoresorcinol, comprises the following steps:

[0038] (1) Dissolve 20 millimoles of concentrated sulfuric acid in 150 milliliters of methanol to obtain methanolic sulfuric acid solution A;

[0039] (2) 10 mmoles of resorcinol and 30 mmoles of potassium iodide are added in batches to solution A under stirring, then heated to 50° C., stirring and dripping 60 mmoles of a mass fraction of 30% hydrogen peroxide solution, After the dropwise addition, react at 50-54°C for 2 hours;

[0040] (3) Cool down to room temperature, vacuum precipitation under stirring, pour the residual liquid into cold water at 5-10°C, and precipitate 4.84 grams of crude product;

[0041] (4) Recrystallized from tetrachloroethylene to obtain white crystal 2,4,6-triiodoresorcinol.

[0042] (5) The conversion rate of the whole reaction is 100%. The final product yield was 96%.

Embodiment 2

[0044] A kind of preparation method of 2,4,6-triiodoresorcinol, comprises the following steps:

[0045] (1) Dissolve 20 millimoles of concentrated sulfuric acid in 100 milliliters of methanol to obtain methanolic sulfuric acid solution A;

[0046](2) 10 mmoles of resorcinol and 30 mmoles of potassium iodide are added in batches to solution A under stirring, then heated to 50° C., stirring and dripping 60 mmoles of a mass fraction of 30% hydrogen peroxide solution, After the dropwise addition, react at 50-54°C for 1 hour;

[0047] (3) Cool down to room temperature, vacuum precipitation under stirring, pour the residue into cold water at 5-10°C, and precipitate 4.82 grams of crude product;

[0048] (4) Recrystallized from tetrachloroethylene to obtain white crystal 2,4,6-triiodoresorcinol.

[0049] (5) The conversion rate of the whole reaction is 99%. The final product yield was 93.2%.

Embodiment 3

[0051] A kind of preparation method of 2,4,6-triiodoresorcinol, comprises the following steps:

[0052] (1) Dissolve 20 millimoles of concentrated sulfuric acid in 200 milliliters of methanol to obtain methanolic sulfuric acid solution A;

[0053] (2) 10 mmoles of resorcinol and 30 mmoles of potassium iodide are added in batches to solution A under stirring, then heated to 50° C., stirring and dripping 60 mmoles of a mass fraction of 30% hydrogen peroxide solution, After the dropwise addition, react at 50-54°C for 3 hours;

[0054] (3) Cool down to room temperature, vacuum precipitation under stirring, pour the residue into cold water at 5-10°C, and precipitate 4.85 grams of crude product;

[0055] (4) Recrystallized from tetrachloroethylene to obtain white crystal 2,4,6-triiodoresorcinol.

[0056] (5) The conversion rate of the whole reaction is 100%. The final product yield was 94.5%.

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Abstract

The invention relates to the technical field of drug synthesis, in particular to a preparation method of 2,4,6-triiodoresorcinol. The preparation method of the 2,4,6-triiodoresorcinol comprises the following steps: in a sulfuric acid methanol solution, taking resorcinol as a substrate and taking potassium iodide as an iodo-reagent, dropwise adding a hydrogen peroxide aqueous solution, and reactinghigh-activity new atomic iodine which is generated by oxidizing the potassium iodide through hydrogen peroxide with the resorcinol to produce the product. By-products are water and inorganic salt. The method for synthesizing iodophenol is an oxidizing iodination process, in the process, the generated high-activity iodinating agent-iodine chloride is generated in real time, iodination consumptionis implemented in real time, and the by-products of reaction is water and potassium sulphate; and reaction is green, effective, safe and controllable.

Description

technical field [0001] The invention relates to the technical field of drug synthesis, and the specific field is a preparation method of iodophenol. Background technique [0002] Iodophenol is 2,4,6-triiodoresorcine (2,4,6-Triiodoresorcine), which is white fine needle-like crystals. The interest of researchers has generated a lot of research work. Iodine powder has a good inhibitory effect on herpes virus, Microsporum, Candida albicans, Staphylococcus aureus and Corynebacterium diphtheriae, and is a broad-spectrum, antiviral drug. Many diseases are often induced by microorganisms and accompanied by viral and fungal infections, so the therapeutic effect of iodophenol is better than other single-acting drugs. [0003] During the treatment process, iodophenol is non-irritating to the skin and has extremely low toxicity, and its production process has mild reaction conditions and stable yield. Now the production of iodophenol has also formed a certain scale industry. In addi...

Claims

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Application Information

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IPC IPC(8): C07C37/62C07C39/24
CPCC07C37/62C07C39/245
Inventor 顾小焱吴孝兰凌芳刘征宙郭建国
Owner SINOPHARM CHEM REAGENT
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