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Trimethyl halogenosilane preparation method

The technology of trimethylhalosilane and trimethylchlorosilane is applied in the field of preparation of trimethyliodosilane, can solve the problems of high production cost, restricted storage and use, deterioration, etc., and achieves less environmental pollution and low production cost Effect

Active Publication Date: 2015-10-07
ZHEJIANG HAIZHOU PHARMA CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Trimethyliodosilane is active, and it is easy to react with oxygen in the air and deteriorate in the air, which limits its preservation and use.
Since the preparation process of iodotrimethylsilane in China is relatively single at present, and most of the processes are not perfect, or the production cost is high, it mainly relies on imports. Therefore, the production of localized products to replace imported products has a great impact on the development of the domestic silicon industry. application significance

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0017] Example 1 Preparation of trimethyliodosilane

[0018] In a 500 ml reaction flask, add 54.3 g (0.5 mol) of trimethylchlorosilane, 57 g (0.5 mol) of hydrogen peroxide 30%, 139 g (0.5 mol) of hydroiodic acid, phase transfer catalyst tetrabutylammonium iodide 26 g, heat up to 10°C, stir for 1 hour, then heat up to 50°C, stir for 3 hours, let stand, use a rectifying device to collect 66.4 g of 105-107°C fraction, with a yield of 66.4%.

Embodiment 2

[0019] Example 2 Preparation of trimethyliodosilane

[0020] In a 500 ml reaction flask, add 54.3 g (0.5 mol) of trimethylchlorosilane, 86 g (0.75 mol) of hydrogen peroxide 30%, 174 g (0.75 mol) of hydroiodic acid, phase transfer catalyst tributylbenzyl iodide 63 g of ammonium chloride was heated to 20°C, stirred for 2 hours, then heated to 60°C, stirred for 4 hours, left to stand, and a rectifying device was used to collect 68.8 g of 105-107°C fraction with a yield of 68.8%.

Embodiment 3

[0021] Example 3 Preparation of trimethylbromosilane

[0022] In a 500 ml reaction flask, add 54.3 g (0.5 mol) of trimethylchlorosilane, 57 g (0.5 mol) of hydrogen peroxide 30%, 85 g (0.5 mol) of hydrobromic acid, phase transfer catalyst trimethyloctyl bromide 26 g of ammonium chloride was heated to 10°C, stirred for 1 hour, then heated to 50°C, stirred for 3 hours, left to stand, and a rectifying device was used to collect 48.8 g of 78-80°C fraction with a yield of 63.8%.

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Abstract

The invention discloses a trimethyl halogenosilane preparation method. The trimethyl halogenosilane preparation method is characterized in that trimethyl halogenosilane, hydrogen peroxide and hydroiodic acid or hydrobromic acid are used as raw materials to be subjected to reaction for 1-6 h at the temperature ranging from 10 DEG C to 80 DEG C under the action of phase transfer catalyst, trimethyl silicon iodide(bromine) is obtained through postprocessing, and the structural formula (I) of the phase transfer catalyst is shown in the specification, wherein R1, R2, R3 and R4 are alkyl or alkyl substitution aryl with the carbon number being 1-18, and X is iodide or bromine.

Description

technical field [0001] The present invention relates to a new preparation method of trimethyl iodide (bromo) silane. Background technique [0002] Trimethylhalosilane is widely used in the field of drug synthesis and organic synthesis. In drug synthesis, trimethyliodosilane is often used as a protective reagent for functional groups such as hydroxyl groups, especially in the fourth generation of cephalosporins such as cefepime, cephalosporin It is widely used in the synthesis of pirox. Trimethyliodosilane is active and easy to react with oxygen in the air to deteriorate, which limits its storage and use. Since the preparation process of trimethyliodosilane in China is relatively simple, and most of the processes are not perfect, or the production cost is high, it mainly depends on imports. Therefore, the production of domestically produced products instead of imported products has a great impact on the development of the domestic silicon industry. application meaning. [...

Claims

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Application Information

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IPC IPC(8): C07F7/12
Inventor 陈昌略王必伟徐大国
Owner ZHEJIANG HAIZHOU PHARMA CO LTD
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