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A kind of method for preparing iodotrimethylsilane

A technology for trimethyliodosilane and trimethylchlorosilane is applied in the field of preparing trimethyliodosilane, 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: 2017-11-03
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 above-mentioned existing method for preparing iodotrimethylsilane, and provide a method for preparing iodotrimethylsilane

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0023] 1) A 250ml three-necked flask, equipped with a feeding funnel, a nitrogen conduit and a reflux condenser, opened the nitrogen purge, and mixed 17.4g of anion exchange resin (201×4(711) strong basic styrene type I anion exchange resin) and 26ml of water (1.4mol) into a three-necked flask, start stirring, heat up to 45°C, add 43.4g (400mmol) of trimethylchlorosilane, add trimethylchlorosilane, heat up to 75°C, stir for 2.5 hours, distill at atmospheric pressure, Collect 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) A 250ml three-neck flask, equipped with a feeding funnel, a nitrogen conduit and a reflux condenser, opened the nitrogen purge, and added step 1) 16.2g (100mmol) of hexamethyldisiloxane and 4.9g (180mmol) of aluminum powder, with an average particl...

Embodiment 2

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

[0027] 1) A 250ml three-neck flask, equipped with a feeding funnel, a nitrogen conduit and a reflux condenser, turned on the nitrogen purge, and added 19.4g of anion exchange resin (D201 macroporous strongly basic styrene-based anion exchange resin) and 23ml (1.2mol) of water Put it 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 and stir for 1.5 hours, distill at normal pressure, collect 99-100°C The fraction 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-neck flask, equipped with an addition funnel, a nitrogen conduit and a reflux condenser, opened the nitrogen purge, added 16.2g (100mmol) of hexamethyldisiloxane and 4g (150mmol, average particle size: 30μm) of alum...

Embodiment 3

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

[0031] 1) A 250ml three-necked flask, equipped with a feeding funnel, a nitrogen conduit and a reflux condenser, turned on the nitrogen purge, and added 15.2g of anion exchange resin (303 weakly basic epoxy anion exchange resin) and 30ml (1.6mol) of water into 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 at 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) A 250ml three-neck flask, equipped with an addition funnel, a nitrogen conduit and a reflux condenser, turned on the nitrogen purge, added 16.2g (100mmol) of hexamethyldisiloxane and 4.3g (160mmol, average particle size of 50μm) of aluminum powder, Star...

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Abstract

The invention discloses a method for preparing iodotrimethylsilane, which comprises the following steps: 1) in the presence of protective gas, add anion exchange resin and water into a reaction vessel, start stirring, raise the temperature to 45°C, add Trimethylchlorosilane, after adding trimethylchlorosilane, heat up to 65-75°C and stir for 1.5-3 hours, distill at atmospheric pressure, collect fractions at 99-100°C, dry with anhydrous sodium sulfate, filter to obtain hexamethyl Disiloxane; 2) In the presence of protective gas, add hexamethyldisiloxane and aluminum powder into another reaction vessel, start stirring, heat up to 55°C, and then add iodine element, after the addition of iodine element is completed The temperature of the bath was raised to 120-140°C, the reaction was refluxed for 2-3 hours, the device was changed to a distillation device, distillation was performed under normal pressure, and fractions at 106-107°C were collected to obtain iodotrimethylsilane. The method can improve the yield of iodotrimethylsilane, has simple operation and mild conditions, and is suitable for large-scale production and popularization.

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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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/12C07F7/08
Inventor 刘行仁欧阳征鹏
Owner 刘行仁
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