Continuous synthetic method for azidotrimethylsilane

A technology of trimethylsilyl, chemical synthesis, applied in chemical instruments and methods, compounds of Group 4/14 elements of the periodic table, organic chemistry, etc., can solve the problems of unstable product quality, poor reaction safety, etc. Improve safety and product quality, short response time and stable product performance

Active Publication Date: 2019-02-05
ASYMCHEM LAB TIANJIN
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AI Technical Summary

Problems solved by technology

[0007] The main purpose of the present invention is to provide a continuous synthesis method of trimethylsilyl azide, so as to solve

Method used

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preparation example Construction

[0020] As described in the background technology, the existing synthetic methods are all batch reactions, which have the problems of unstable product quality and poor reaction safety. In order to solve the above technical problems, the application provides a trimethylsilyl azide (TMSN 3 ), the continuous synthesis method comprises: under a protective atmosphere, trimethylsilyl chloride (TMSCl) and azide are continuously transported as reaction raw materials to a continuous synthesis device for nucleophilic substitution Reaction, trimethylsilyl azide is obtained, and trimethylsilyl azide is discharged continuously, and the protective atmosphere is selected from nitrogen and / or inert gas.

[0021] This application adopts a continuous synthesis process to synthesize trimethylsilyl azide, the reaction time required for the whole reaction process is short, the output is large, and the product performance is relatively stable. At the same time, since the application adopts a contin...

Embodiment 1

[0034] Dissolve trimethylsilyl chloride (TMSCl, 217.3g, 2.0mol) in trimethylsilyl azide (TMSN 3 , 217.3g) after stirring evenly, use pump A to pump into the three-stage CSTR at a speed of 1.19g / min.

[0035] NaN 3(136.5g, 2.1mol) was added into the third-stage CSTR through a solid feeder at a rate of 0.36g / min, and the system passed through the residence time of the third-stage CSTR for a total of 5h. Use an external oil bath temperature control device to control the temperature in the CSTR at 35° C. to carry out the nucleophilic reaction and obtain a nucleophilic reaction product system.

[0036] The last level of CSTR is connected to the continuous filter device to filter the nucleophilic reaction product system, and the filtrate is collected to obtain 214.3g of colorless transparent liquid product (not included in solvent TMSN 3 ), the yield is 93.0wt%, and the gas chromatography purity is 97.8%.

Embodiment 2

[0038] The difference from Example 1 is that TMSN is not used 3 As the solvent, use Dawson's oil as the solvent instead.

[0039] After dissolving TMSCl (217.3g, 2.0mol) in Dawson oil (217.3g) and stirring evenly, use pump A to pump it into the three-stage CSTR at a speed of 1.19g / min.

[0040] NaN 3 (136.5g, 2.1mol) was added into the third-stage CSTR through a solid feeder at a rate of 0.36g / min, and the system passed through the residence time of the third-stage CSTR for a total of 5h. The temperature in the three-stage CSTR was controlled at 35°C by using an external oil bath temperature control device to carry out the nucleophilic reaction and obtain a nucleophilic reaction product system.

[0041] The last stage of CSTR is connected to a continuous filtration device, and the obtained filtrate is distilled under reduced pressure (40-60mBar), and a fraction at 40-50°C is obtained, 209.7g of a colorless and transparent liquid product, the yield is 91.0wt%, and the gas chr...

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Abstract

The invention provides a continuous synthetic method for azidotrimethylsilane. The continuous synthetic method comprises the following steps of at a protective atmosphere, continuously conveying trimethyl-chlorosilane and an azide as reaction raw materials to a continuous synthesizer to perform nucleophilic substitution reaction to obtain the azidotrimethylsilane, and continuously discharging theazidotrimethylsilane, wherein the protective atmosphere is selected from nitrogen and/or inert gas. In the continuous synthetic method, by adopting a continuous synthetic technology to synthesize theazidotrimethylsilane; and in the whole reaction process, the required reaction time is short, the yield is large, and the performance of a product is stable. Meanwhile, as the invention adopts the continuous synthetic technology, the reaction heat can be timely brought away from the continuous synthesizer at any time, so that lowering of the risk of heat accumulation when scale reaction is amplified is facilitated, operation is simplified, and the safety of continuous batch production is improved. Therefore, by adopting the continuous synthetic technology provided by the invention to prepare the azidotrimethylsilane, improvement on safety of the whole reaction process and quality of the product is facilitated.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a continuous synthesis method of trimethylsilyl azide. Background technique [0002] Trimethylsilyl azide is a very important intermediate in organic synthesis, widely used in the synthesis of amination reagents, azidation reagents and nitrogen heterocyclic compounds. [0003] The existing literature provides a preparation method of trimethylsilyl azide, the preparation method comprising: using decahydronaphthalene as a solvent, adding trimethylchlorosilane and sodium azide to ion exchange under the condition of 60°C The reaction was carried out in resin XAD-4 to obtain the product trimethylsilyl azide. In this reaction, the yield of trimethylsilyl azide is relatively low, only 82%. [0004] Another existing document reports a preparation method of trimethylsilyl azide, which preparation method comprises: using trimethylchlorosilane and sodium azide as raw materials, and using ...

Claims

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Application Information

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IPC IPC(8): C07F7/10
CPCC07F7/10
Inventor 洪浩卢江平张恩选刘志清李超杨思航
Owner ASYMCHEM LAB TIANJIN
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