Method for preparing triethyl silicane

A technology of triethyl and trichlorosilane, which is applied in the direction of silicon organic compounds, can solve the problems of harsh reaction conditions, high cost, and low yield, and achieve the effect of mild reaction conditions, low cost, and less pollution

Inactive Publication Date: 2011-05-11
河南豫辰药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a preparation method of triethylsilane, which overcomes the defects of harsh reaction conditions, high cost or need for purification and low yield in the existing method, and is convenient for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In a clean and dry reaction bottle, add 14g of magnesium powder, 66g of bromoethane, 6g of ether, 80g of trimethylbenzene, iodine or the previous batch of Grignard reagent, control the temperature at 80-100°C to make ethylmagnesium bromide solution, and then control Add dropwise a mixture of 21 g of trimethylbenzene and 18 g of trichlorosilane at a temperature of 0-60° C., keep the temperature after the dropwise addition, and end the reaction.

[0021] Add the reaction solution dropwise into the ice-water mixture, adjust the pH to 3 with reagent hydrochloric acid, control the temperature below 40°C, after the drop is complete, let it stand for stratification, hydrolyze the organic layer, separate the layers, distill the organic layer, collect and distill at 107-109°C Products, more than 99% of triethylsilane products.

Embodiment 2

[0023] In a clean and dry reaction bottle, add 13g of magnesium powder, 42g of ethyl chloride, 7g of ether, 108g of trimethylbenzene, iodine or the previous batch of Grignard reagent, control the temperature at 80-100°C to make ethylmagnesium chloride solution, and then control the temperature Add 20 g of trichlorosilane dropwise at 0-60°C, keep warm after the dropwise addition, and end the reaction.

[0024] Add the reaction solution dropwise into the ice-water mixture, adjust the pH to 6 with reagent hydrochloric acid, control the temperature below 40°C, after the drop is complete, let it stand for stratification, hydrolyze the organic layer, separate the layers, distill the organic layer, collect and distill at 107-109°C Products, more than 99% of triethylsilane products.

Embodiment 3

[0026] In a clean and dry reaction bottle, add 14g of magnesium powder, 81g of bromoethane, 5g of methyl tert-butyl ether, 77g of xylene, iodine or the previous batch of Grignard reagent, and control the temperature at 60-80°C to make ethyl bromide Magnesium chloride solution, then add dropwise a mixture of 20g xylene and 22g trichlorosilane at a temperature of 0-60°C, keep the temperature after the dropwise addition, and end the reaction.

[0027] Add the reaction solution dropwise into the ice-water mixture, adjust the pH to 3 with reagent hydrochloric acid, control the temperature below 40°C, after the drop is complete, let stand to separate and separate, the organic layer is hydrolyzed, separated, and distilled, and the distillate at 107-109°C is collected to obtain More than 99% triethylsilane products.

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Abstract

The invention belongs to the field of the preparation of medicinal intermediates, and particularly relates to a method for preparing triethyl silicane. The method comprises the following steps of: performing a condensation reaction of trichlorosilane, halothane and magnesium powder in an alkane or arene organic solvent containing an ether catalyst, and purifying a reaction production to obtain the triethyl silicane. By the method for preparing the triethyl silicane, the obtained product has fewer impurities, and the product content is over 99 percent; and the preparation method has low cost, less pollution and mild reaction condition, is easy and convenient to operate, and is convenient for industrial production.

Description

(1) Technical field [0001] The invention belongs to the field of preparation of pharmaceutical intermediates, in particular to the preparation of triethylsilane. (2) Background technology [0002] Triethylsilane is a general-purpose silane-based reducing agent, which is widely used in organic synthesis and is also an important raw material for pharmaceutical intermediates. The current preparation method of triethylsilane is found in GB 795,185 and GB781,533. GB 795,185 describes a synthesis method for preparing triethylsilane by hydrogenation of triethylfluorosilane in the presence of sodium. The reaction temperature of this method reaches 300° C., and the yield reaches 90%. However, this method has high reaction temperature and high price of triethylfluorosilane, which is not suitable for industrial production. GB 781,533 discloses a method for preparing triethylsilane by reacting triethylfluorosilane and diethylaluminumsilane, but the method obtains a mixture of triethyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08
Inventor 钱庆生罗明路明蔡迎雷马杰
Owner 河南豫辰药业股份有限公司
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