Process for synthesizing iodotrimethylsilane

A technology of trimethyliodosilane and a synthesis method, which is applied in chemical instruments and methods, compounds of Group 4/14 elements of the periodic table, organic chemistry, etc., can solve problems such as unfavorable ceftazidime synthesis, side effects, etc. The effect of reducing side effects

Active Publication Date: 2007-05-16
扬州三友合成化工有限公司
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Problems solved by technology

However, the trimethyl iodosilane that has been sold at present is synthesized by a one-step method in the production process, and nuclear magnetic mass spectrometry proves that there are many l

Method used

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Embodiment Construction

[0018] Steps:

[0019] 1. Preparation of crude iodotrimethylsilane:

[0020] Add 13.5 kg (500 mol) of aluminum powder and 64.8 kg (400 mol) of hexamethyldisiloxane into the dry reaction kettle, start the mixer, heat the oil bath, raise the temperature of the materials in the kettle to 55-65 ° C, and start adding iodine. After the reaction is initiated, control the temperature at 65-75°C, slowly add 157.5kg (620 mol) of refined iodine in batches within 1 hour, gradually raise the temperature to 140±10°C, reflux for 1.5-2 hours, change to a distillation device, and distill at atmospheric pressure , collecting fractions at 100-150° C. to obtain 134.8 kg (84.25%) of crude iodotrimethylsilane.

[0021] The temperature in the kettle is 210-220°C, stop the distillation, lower the temperature to 140±10°C, add 100L of high-boiling point hydrocarbon solvent (such as xylene or paraffin oil, etc.), lower the temperature to 60-70°C, add 20% KOH solution 400kg After the addition, measure ...

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Abstract

The invention discloses a synthesizing method of trimethyl iodine silane, which comprises the following steps: adding aluminium, hexamethyldisilazane and iodine in the autoclave; distilling; obtaining the rough product of trimethyl iodine silane; placing rough product in the distilling autoclave; adding copper powder; heating; collecting fraction; obtaining the refined product.

Description

technical field [0001] The invention relates to a synthesis method of chemical products. Background technique [0002] Usually, iodotrimethylsilane can form organosilicon reagents that are easily dissociated derivatives with compounds containing hydroxyl, carboxyl and amino groups. These reagents are often used to protect hydroxyl groups in organic synthesis. The application of iodotrimethylsilane is very wide. Play an important role in organic reactions. The demand for iodotrimethylsilane as an intermediate in the production of ceftazidime is increasing year by year. There are almost no domestic manufacturers of trimethyl iodide silicon in batches, and all the trimethyl iodide silicon in circulation are either produced in small quantities by domestic laboratories or imported from abroad. [0003] There are more than ten kinds of synthesis methods of iodotrimethylsilane, and the more practical and industrialized synthesis methods are the reaction of hexamethyldisiloxane, i...

Claims

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Application Information

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IPC IPC(8): C07F7/12
Inventor 李明成张扬张才山陆灯宏
Owner 扬州三友合成化工有限公司
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