Trimethyliodosilane preparation method

A technology for trimethyl iodide silane and trimethyl chlorosilane is applied in the field of preparing trimethyl iodide silane, which can solve the problems of many by-products and low yield, and achieve the effects of less impurities, high yield and simple purification.

Inactive Publication Date: 2016-02-03
刘行仁
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the defects of low yield and many by-products in the abov

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0021] Example 1

[0022] A method for preparing trimethylsilyl iodide, the method comprising the following steps:

[0023] 1) 250ml three-necked flask, equipped with feeding funnel, nitrogen conduit and reflux condenser, turn on nitrogen purge, and add 17.4g of anion exchange resin (201×4(711) strong basic styrene type I anion exchange resin) and 26ml of water (1.4mol) was added to a three-necked flask, stirred, heated to 45°C, added 43.4g (400mmol) of trimethylchlorosilane, added trimethylchlorosilane, heated to 75°C, stirred for 2.5 hours, and distilled at atmospheric pressure. Collect the fractions at 99-100°C, dry with anhydrous sodium sulfate, and filter to obtain 30.5 g of hexamethyldisiloxane with a purity of 99.5% and a yield of 93.8%;

[0024] 2) 250ml three-necked flask, equipment feeding funnel, nitrogen conduit and reflux condenser, turn on nitrogen purge, add step 1) hexamethyldisiloxane 16.2g (100mmol) and aluminum powder 4.9g (180mmol, average particle size is 35μm)...

Example Embodiment

[0025] Example 2

[0026] A method for preparing trimethylsilyl iodide, the method comprising the following steps:

[0027] 1) 250ml three-necked flask, equipment feeding funnel, nitrogen conduit and reflux condenser, open nitrogen purge, add 19.4g anion exchange resin (D201 macroporous strong basic styrene anion exchange resin) and 23ml (1.2mol) water Into a three-necked flask, start stirring, heat up to 45°C, add 43.4g (400mmol) of trimethylchlorosilane, add trimethylchlorosilane, heat up to 70°C, stir for 1.5 hours, distill under normal pressure, collect 99-100°C The distillate was dried with anhydrous sodium sulfate and filtered to obtain 29.8 g of hexamethyldisiloxane with a purity of 99.6% and a yield of 91.7%;

[0028] 2) A 250ml three-necked flask, equipment feeding funnel, nitrogen conduit and reflux condenser, turn on nitrogen purge, add 16.2g (100mmol) of hexamethyldisiloxane and 4g (150mmol, average particle size of 30μm) of aluminum powder, start Magnetically stir, hea...

Example Embodiment

[0029] Example 3

[0030] A method for preparing trimethylsilyl iodide, the method comprising the following steps:

[0031] 1) 250ml three-necked flask, equipped with feeding funnel, nitrogen conduit and reflux condenser, turn on nitrogen purge, add 15.2g of anion exchange resin (303 weakly basic epoxy anion exchange resin) and 30ml (1.6mol) of water to the three-necked flask In the flask, start stirring, heat up to 45°C, add 43.4g (400mmol) of trimethylchlorosilane, add trimethylchlorosilane, heat up to 65°C and stir for 2 hours, distill under normal pressure, collect 99-100°C fractions, Dry with anhydrous sodium sulfate and filter to obtain 29.5 g of hexamethyldisiloxane with a purity of 99.8% and a yield of 90.9%;

[0032] 2) 250ml three-necked flask, equipped with feeding funnel, nitrogen conduit and reflux condenser, turn on nitrogen purge, add 16.2g (100mmol) of hexamethyldisiloxane and 4.3g (160mmol, average particle size of 50μm) of aluminum powder, Start magnetic stirring,...

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Abstract

The present invention discloses a trimethyliodosilane preparation method comprising the steps of: 1) in the presence of a protective gas, anion exchange resin and water are added into a reaction vessel, then stirring is started, the reaction vessel is heated to 45 DEG C, trimethyl chlorosilane is added, after the trimethylchlorosilane is added, the reaction vessel is heated to 65-75 DEG C and stirred for 1.5-3 hours for reaction, atmospheric distillation is performed, 99-100 DEG C distillate is collected, dried with anhydrous sodium sulfate, and filtered to obtain hexamethyldisiloxane; 2) in the presence of a protective gas, the hexamethyldisiloxane and aluminum powder are added into another reaction vessel, stirring is started, the reaction vessel is heated to 55 DEG C, elemental iodine is added, after completion of the addition of the elemental iodine, the bath temperature is raised to 120-140 DEG C for reaction and refluxing for 2-3 hours, the device is changed into a distillation apparatus for atmospheric distillation, and 106-107 DEG C distillate is collected to obtain the trimethyliodosilane. The method can improve the yield of the trimethyliodosilane, and is simple in operation, mild in conditions, and suitable for mass production and marketing.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a method for preparing iodotrimethylsilane. Background technique [0002] Iodotrimethylsilane is often used as a protective reagent for functional groups such as amino, hydroxyl, and mercapto groups in the field of drug synthesis and organic synthesis. Due to its high activity and mild reaction conditions, it has a wide range of applications, especially in drug synthesis such as cefepime. , Application in the synthesis of cefpirome. [0003] At present, there are many ways to synthesize iodotrimethylsilane. The commonly used synthesis method in industry is to react hexamethyldisiloxane with iodine and aluminum powder to prepare iodotrimethylsilane. Industrially, hexamethyldisiloxane is mainly obtained by hydrolysis of trimethylchlorosilane. Since the reaction system is acidic after hydrolysis, it is often necessary to add an organic or inorganic base as an acid-bindi...

Claims

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Application Information

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IPC IPC(8): C07F7/12C07F7/08
Inventor 吴兴连
Owner 刘行仁
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