Method for preparing iodobenzene diacetate

A technology of iodobenzene diacetate and iodobenzene, which is applied in the field of preparation of oxidant iodobenzene diacetate, which can solve problems affecting the environment, pollution, hidden dangers, etc., and achieve the effects of simple operation, reasonable process and safe production

Active Publication Date: 2009-11-11
上海予利生物科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Iodobenzene diacetate belongs to the organic hypervalent iodine compound, which is a kind of mild, non-toxic oxidizing agent and has strong electrophilic reagent, and the previous heavy metal oxides such as KMnO 4 , CrO 3 Compared with others, it has the advantages of non-pollution and non-toxicity. Traditional heavy metal oxidants will cause pollution after use, affect the environment, and cause waste of resources at the same time.
[0003] The traditional synthesis process of iodobenzene diacetate is prepared by reacting iodobenzene with 40% peracetic acid, and 40% peracetic acid is a strong oxidant, which is explosive and has a high risk in production, storage, transportation and use. There are many hidden dangers, and if you are not careful, explosion accidents will easily occur, which will cause unstable effects on the country, enterprises and employees. Moreover, it is difficult to buy more than 40% peracetic acid in the market. Generally, the supply on the market is in 18-23% concentration, and the preparation of iodobenzene diacetate concentration must be as high as 40% peracetic acid to react
Due to the limitation of factors such as safety, the production scale of this process is very small and the output is very low

Method used

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  • Method for preparing iodobenzene diacetate

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Embodiment 1

[0021] A method for preparing iodobenzene diacetate, the method may further comprise the steps:

[0022] Add 40.8 grams (0.2mol) of iodobenzene to 250 milliliters of glacial acetic acid and 250 milliliters of acetic anhydride, heat to 35-40 degrees, then add 184.8 grams (1.2mol) of sodium perborate tetrahydrate in batches within 30 minutes, and the reaction temperature is maintained at 40-45 degrees, then keep warm at 40-45 degrees and react for 12 hours, then cool to room temperature, add 1500 ml of ice water, precipitate iodobenzene diacetate crude product, recrystallize with glacial acetic acid / petroleum ether to obtain 46 grams, yield 71.4% . Melting point: 158-160°C, content 100.7%.

Embodiment 2

[0024] A method for preparing iodobenzene diacetate on a large scale, the method may further comprise the steps:

[0025] Add 600 grams (2.94mol) of iodobenzene to 4 liters of glacial acetic acid and 2 liters of acetic anhydride, heat to 35-40 degrees, then add 1400 grams (9.1mol) of sodium perborate tetrahydrate in batches within 40-60 minutes, the reaction temperature Maintain at 40-45 degrees, then keep warm at 40-45 degrees and react for 6 hours, then cool to room temperature, add 12 liters of ice water, precipitate iodobenzene diacetate crude product, recrystallize with glacial acetic acid / petroleum ether to obtain 635 grams, yield 66.8%. Melting point: 160-164°C, content 99.2%.

Embodiment 3

[0027] A kind of preparation method of iodobenzene diacetate, this method takes sodium perborate tetrahydrate as raw material, is made into acylation reagent with glacial acetic acid / acetic anhydride mixed solution, the volume of glacial acetic acid and acetic anhydride in glacial acetic acid / acetic anhydride mixed solution Ratio is 2: 1, sodium perborate tetrahydrate is fed in batches within 15 minutes, and acylation reaction occurs with iodobenzene, wherein the mol ratio of sodium perborate tetrahydrate and iodobenzene is 3: 1, and the reaction temperature is 30°C, The reaction time was 4 hours. After the reaction was completed, ice water with 16 times the volume of iodobenzene was added to obtain the crude product of iodobenzene diacetate, which was then recrystallized by glacial acetic acid / petroleum ether to obtain iodobenzene diacetate.

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Abstract

The invention relates to a method for preparing iodobenzene diacetate, which comprises the following steps: using tetrahydrate sodium perborate as a raw material to perform acylation reaction with iodobenzene in the presence of a glacial acetic acid / acetic anhydride mixed solution, wherein the molar ratio of the tetrahydrate sodium perborate to the iodobenzene is 3-10:1, the reaction temperature is between 30 and 45 DEG C, and the reaction time is between 4 and 24 hours; after the reaction, adding ice water to obtain a crude product of the iodobenzene diacetate; and performing recrystallization to obtain the iodobenzene diacetate. Compared with the prior art, the method has the advantages of reasonable process, simple operation and safe production, is suitable for industrial mass production, and provides a favorable condition for producing the iodobenzene diacetate industrially.

Description

technical field [0001] The invention relates to an organic iodine oxidant, in particular to a method for preparing the oxidant iodobenzene diacetate. Background technique [0002] Iodobenzene diacetate belongs to the organic hypervalent iodine compound, which is a kind of mild, non-toxic oxidizing agent and has strong electrophilic reagent, and the previous heavy metal oxides such as KMnO 4 , CrO 3 Compared with others, it has the advantages of non-pollution and non-toxicity. Traditional heavy metal oxidants will cause pollution after use, which will affect the environment and cause waste of resources. Iodobenzene diacetate is used in pharmaceutical industries and has good selective oxidation characteristics, and has been more and more widely used in recent years. For example, the synthesis of the latest oral lung cancer treatment drug topotecan, anti-inflammatory analgesic drug naproxen, antidepressant fluoxetine, influenza drug oseltamivir (Tamiflu) for bird flu, and ant...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C71/00
Inventor 俞建新顾建良费巧龙张林宝
Owner 上海予利生物科技股份有限公司
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