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Iodotrimethylsilane preparation method

A technology of iodotrimethylsilane and hexamethyldisiloxane, which is applied in the field of preparation of iodotrimethylsilane, can solve the problems of slow reaction, low yield, deterioration, etc., and achieve fast reaction speed and high yield Effect

Active Publication Date: 2015-09-23
山东博苑医药化学股份有限公司
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  • Summary
  • 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, which limits its storage and use.
The yield of this method is low, the crude yield of the reaction is only 84.25%, and the refined yield is only 78.49%, that is, the total yield of pure iodotrimethylsilane prepared by this method is only 84.25%×78.49%=66.13%; the refining step , the amount of copper powder is large, which is not conducive to the reduction of production costs
The operation steps of this method include adding refined iodine in batches. Because iodine has a high vapor pressure, it is easy to sublime, has a pungent smell, and is easy to condense after sublimation. It is toxic and corrosive, so this step of operation pollutes the environment and is serious. hazard operator
Iodine and aluminum powder are both solids, and the reaction between solid and solid is slow and unstable. The aluminum triiodide solid generated by the reaction of iodine and aluminum powder covers the surface of iodine and aluminum powder, hindering further reaction. very low rate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 8.6 g of ultrafine aluminum powder (325 mesh) and 16.2 g of hexamethyldisiloxane into a 250 mL four-neck flask. In the constant pressure dropping funnel, first add a layer of rectification column packing glass spring, then 76.2 g of elemental iodine and 16.2 g of hexamethyldisiloxane, the reaction system is evacuated and nitrogen is changed, and this is repeated three times. Stirring was started, the temperature was raised to 60°C, and a solution of iodine in hexamethyldisiloxane was added dropwise. After the dropwise addition is completed, the external temperature is raised to 130° C. to reflux, and the steam is cooled and enters the constant-pressure dropping funnel to dissolve the undissolved iodine in the constant-pressure dropping funnel. After the iodine is completely dissolved and added dropwise to the reaction system, the reaction is completed for another 1.5 hours. Stop heating, lower the temperature to below 30°C, change the reaction device to a distillat...

Embodiment 2

[0025] Add 8.6 g of ultrafine aluminum powder (800 mesh) and 16.2 g of hexamethyldisiloxane into a 250 mL four-necked bottle. In the constant pressure dropping funnel, first add a layer of rectification column packing glass spring, then 76.2 g of elemental iodine and 16.2 g of hexamethyldisiloxane, the reaction system is evacuated and nitrogen is changed, and this is repeated three times. Stirring was started, the temperature was raised to 60°C, and a solution of iodine in hexamethyldisiloxane was added dropwise. After the dropwise addition is completed, the external temperature is raised to 130° C. to reflux, and the steam is cooled and enters the constant-pressure dropping funnel to dissolve the undissolved iodine in the constant-pressure dropping funnel. After the iodine is completely dissolved and added dropwise to the reaction system, react for another 1 hour until the reaction is complete. Stop heating, lower the temperature to below 30°C, change the reaction device to ...

Embodiment 3

[0028] Add 8.6 g of ordinary aluminum powder (40 mesh) and 16.2 g of hexamethyldisiloxane into a 250 mL four-necked bottle. In the constant pressure dropping funnel, first add a layer of rectification column packing glass spring, then 76.2 g of elemental iodine and 16.2 g of hexamethyldisiloxane, the reaction system is evacuated and nitrogen is changed, and this is repeated three times. Stirring was started, the temperature was raised to 60°C, and a solution of iodine in hexamethyldisiloxane was added dropwise. After the dropwise addition is completed, the external temperature is raised to 130° C. to reflux, and the steam is cooled and enters the constant-pressure dropping funnel to dissolve the undissolved iodine in the constant-pressure dropping funnel. After the iodine is completely dissolved and added dropwise to the reaction system, the reaction is completed for another 3 hours. Stop heating, lower the temperature to below 30°C, change the reaction device to a distillati...

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Abstract

The invention provides an iodotrimethylsilane preparation method. The preparation method comprises the following steps that superfine aluminum power and half hexamethyldisiloxane are put in a reaction flask, elementary substance iodine and half hexamethyldisiloxane are put in a constant pressure dropping funnel, vacuumizing and nitrogen replacing are performed on a reaction system, and all the steps are repeated for three times; stirring is started, the temperature rises to 60 DEG C, and hexamethyldisiloxane solutions of the iodine are dropwise added; after dropwise adding is finished, the outer temperature rises to 130 DEG C for backflow, and therefore after being cooled, steam enters the constant pressure dropping funnel to dissolve the undissolved iodine in the constant pressure dropping funnel; after the iodine is dissolved completely and dropwise added in the reaction system, reaction is performed for 2 hours until the reaction is complete; heating is stopped, the temperature is cooled below 30 DEG C, a reaction device is changed into a distillation device to collect main distillate fractions, and then colorless liquid iodotrimethylsilane competitive products are obtained.

Description

technical field [0001] The invention relates to a preparation method of iodotrimethylsilane, which belongs to the field of chemical synthesis. Background technique [0002] Iodotrimethylsilane is widely used in the fields 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 cephalosporins such as cefepime and cefepime. Luo's synthetic process has been widely used. Iodotrimethylsilane is active in nature and easily reacts with oxygen in the air to deteriorate, which limits its storage and use. [0003] There are more than 10 synthetic methods of iodotrimethylsilane, and the more practical and industrialized synthetic methods are the reaction of hexamethyldisiloxane with iodine and aluminum powder, and the reaction of hexamethyldisilane with iodine. The trimethyliodosilane currently on the market contains a lot of low-boiling imp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/12
Inventor 李成林于国清汪清民
Owner 山东博苑医药化学股份有限公司
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