CN103554167A - Method for preparing trimethylsilyl azide - Google Patents
Method for preparing trimethylsilyl azide Download PDFInfo
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- CN103554167A CN103554167A CN201310532966.5A CN201310532966A CN103554167A CN 103554167 A CN103554167 A CN 103554167A CN 201310532966 A CN201310532966 A CN 201310532966A CN 103554167 A CN103554167 A CN 103554167A
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- silicon
- azide
- trimethyl azide
- trimethyl
- preparation
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Abstract
The invention discloses a method for preparing trimethylsilyl azide. The method comprises steps of firstly, adding DMF (dimethyl formamide) into sodium azide, wherein the proportion of DMF is less than 1/4(g/ml); secondly, stirring through a stirring rod for dissolving; thirdly, slowly dropping trimethylchloro silane; fourthly, standing sodium azide for 24 hours at room temperature; fifthly, simply distilling at normal pressure, and collecting 90-100 DEG C former cut fraction to obtain trimethylsilyl azide; sixthly, rectifying. The method for preparing thrimethylsilyl azide is easy to control, the yield of sodium azide is 150% by weight, the product is colourless and transparent liquid, and the method is applicable to industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of silication reagent, be specifically related to a kind of preparation method of trimethyl azide silicon.
Background technology
Trimethyl azide silicon is a kind of important silication reagent, is widely used in aminating agent, nitrine agent or heterogeneous ring compound synthetic, because trimethyl azide silicon synthetic reaction condition is gentle, is easy to control, and is applicable to industrialized production; Therefore this produce market demand progressively increases, and has good development prospect.
In the existing method of preparing trimethyl azide silicon, generally need to pass through all kinds of SOLVENTS, the additive such as promotor, phase-transfer catalyst impels the successful preparation of trimethyl azide silicon, because the quantity of various raw materials, character etc. influence each other, in actual production, be not easy to control, so the quality of trimethyl azide silicon and yield are all difficult to be guaranteed; And production cost is higher.
Summary of the invention
For addressing the above problem, the object of the invention is to provide a kind of preparation method of new trimethyl azide silicon, makes easily to control in trimethyl azide silicon preparation process, has also improved quality and the yield of trimethyl azide silicon simultaneously.
For achieving the above object, the technical solution adopted in the present invention is:
A preparation method for trimethyl azide silicon, the first step, adds DMF to sodiumazide, and adding proportion is less than 1/4 (g/ml); Second step, carries out stirring and dissolving by stirring rod; The 3rd step, slowly drips trimethylammonium silicon chlorides; The 4th step, to the sodiumazide timing dropwising, keeps room temperature 24 hours; The 5th step, normal pressure simple distillation, collects the trimethyl azide silicon that 90-100 ° is front-end volatiles; The 6th step, carries out rectifying.
As preferably, the trimethyl azide silicon of described front-end volatiles can be applied mechanically down batch when trimethylammonium silicon chlorides.
Beneficial effect:
The preparation method of trimethyl azide silicon of the present invention, has solved in prior art and has been not easy to control about trimethyl azide silicon preparation process, the problem that the quality of trimethyl azide silicon and yield do not reach promising result simultaneously; Having proposed a kind of preparation method of new trimethyl azide silicon, used reaction after method of the present invention to be very easy to control, is 150% to sodiumazide weight yield, and product appearance is achromaticity and clarification liquid, is well suited for suitability for industrialized production.
Embodiment
The preparation method of trimethyl azide silicon of the present invention; The first step, adds DMF to sodiumazide, and adding proportion is less than 1/4 (g/ml); Second step, carries out stirring and dissolving by stirring rod; The 3rd step, slowly drips trimethylammonium silicon chlorides; The 4th step, to the sodiumazide timing dropwising, keeps room temperature 24 hours: the 5th step, and normal pressure simple distillation, collects the trimethyl azide silicon that 90-100 ° is front-end volatiles; The 6th step, carries out rectifying.As preferably, the trimethyl azide silicon of described front-end volatiles can be applied mechanically down batch when trimethylammonium silicon chlorides.
Embodiment 1
Get sodiumazide 100g, add DMF400ml stirring and dissolving, under room temperature, start to drip trimethylammonium silicon chlorides 200ml, insulation reaction 20 hours, simple distillation, collects 95-100 degree cut, obtains trimethyl azide silicon 90g, content 90%; Trimethyl azide silicone content 78% in 80-95 degree front-end volatiles; Respectively rectifying, can obtain cut more than 98% product and 90%; Front-end volatiles partly overlap for reaction, finally can obtain the trimethyl azide SiClx for sodiumazide weight yield 150%, and content is more than 98%.
The preparation method of trimethyl azide silicon of the present invention, reaction is very easy to control, and to sodiumazide weight yield, is 150%, and product appearance is achromaticity and clarification liquid, is well suited for suitability for industrialized production.
Embodiment recited above is described the preferred embodiment of the present invention, not the spirit and scope of the present invention is limited.Do not departing under the prerequisite of design concept of the present invention; various modification and improvement that this area ordinary person makes technical scheme of the present invention; all should drop into protection scope of the present invention, the technology contents that the present invention asks for protection, is all documented in claims.
Claims (2)
1. a preparation method for trimethyl azide silicon, is characterized in that: the first step, add DMF to sodiumazide, and adding proportion is less than 1/4 (g/ml); Second step, carries out stirring and dissolving by stirring rod; The 3rd step, slowly drips trimethylammonium silicon chlorides; The 4th step, to the sodiumazide timing dropwising, keeps room temperature 24 hours; The 5th step, normal pressure simple distillation, collects the trimethyl azide silicon that 90-100 ° is front-end volatiles; The 6th step, carries out rectifying.
2. the preparation method of trimethyl azide silicon according to claim 1, is characterized in that: the trimethyl azide silicon of described front-end volatiles can be applied mechanically down and criticize when trimethylammonium silicon chlorides.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310532966.5A CN103554167A (en) | 2013-10-29 | 2013-10-29 | Method for preparing trimethylsilyl azide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310532966.5A CN103554167A (en) | 2013-10-29 | 2013-10-29 | Method for preparing trimethylsilyl azide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103554167A true CN103554167A (en) | 2014-02-05 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310532966.5A Pending CN103554167A (en) | 2013-10-29 | 2013-10-29 | Method for preparing trimethylsilyl azide |
Country Status (1)
| Country | Link |
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| CN (1) | CN103554167A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4426531A (en) * | 1978-12-14 | 1984-01-17 | Dynamit Nobel Aktiengesellschaft | Process for the preparation of 1H-tetrazole-1 compounds using trimethylsilyl azide |
| CN102010381A (en) * | 2009-09-05 | 2011-04-13 | 山东新时代药业有限公司 | Improved preparation method of valsartan |
-
2013
- 2013-10-29 CN CN201310532966.5A patent/CN103554167A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4426531A (en) * | 1978-12-14 | 1984-01-17 | Dynamit Nobel Aktiengesellschaft | Process for the preparation of 1H-tetrazole-1 compounds using trimethylsilyl azide |
| CN102010381A (en) * | 2009-09-05 | 2011-04-13 | 山东新时代药业有限公司 | Improved preparation method of valsartan |
Non-Patent Citations (4)
| Title |
|---|
| KARAVAI, V. P.等: "A simple synthesis of trimethylsilyl azide", 《METALLOORGANICHESKAYA KHIMIYA》 * |
| KAZUAKI SUKATA: "Efficient Synthesis of Silyl Azides Using Sodium Azide Impregnated on Amberlite XAD Resin", 《J. ORG. CHEM.》 * |
| STEPHEN S. WASHBURNE等: "FACILE PREPARATION OF SILYL AZIDES WITH DIPOLAR APROTIC SOLVENTS", 《J. ORGANOMETAL. CHEM.》 * |
| 刘洁: "三甲基叠氮硅合成含氮类杂环化合物的研究", 《华东师范大学硕士学位论文》 * |
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Application publication date: 20140205 |
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