CN106928268B - A method of preparing iodotrimethylsilane - Google Patents
A method of preparing iodotrimethylsilane Download PDFInfo
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- CN106928268B CN106928268B CN201710134989.9A CN201710134989A CN106928268B CN 106928268 B CN106928268 B CN 106928268B CN 201710134989 A CN201710134989 A CN 201710134989A CN 106928268 B CN106928268 B CN 106928268B
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- iodotrimethylsilane
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/12—Organo silicon halides
- C07F7/121—Preparation or treatment not provided for in C07F7/14, C07F7/16 or C07F7/20
- C07F7/123—Preparation or treatment not provided for in C07F7/14, C07F7/16 or C07F7/20 by reactions involving the formation of Si-halogen linkages
Abstract
The preparation process of mild, simple for process, safe operation that the present invention relates to a kind of reaction conditions, high income and the few Iodotrimethylsilane of the three wastes, using anhydrous sodium iodide, anhydrous lithium chloride, trim,ethylchlorosilane as raw material, Iodotrimethylsilane is synthesized in dry nitrogen atmosphere.This method changes traditional hexamethyldisilane, hexamethyldisiloxane prepares the complicated technology of iodine silane; reaction condition is mild; safe operation; avoid the danger using high-risk chemical metallic potassium, sodium; also avoiding high temperature simultaneously adds iodine problem, entire production cycle process, output there was only Iodotrimethylsilane product and byproduct sodium chloride; generation without other three wastes, technique are environmentally protective.
Description
Technical field
The present invention relates to a kind of preparation method of chemical products more particularly to a kind of new sides preparing Iodotrimethylsilane
Method belongs to the field of chemical synthesis.
Background technology
Iodotrimethylsilane is in pharmaceutical synthesis and organic synthesis field frequently as functional groups such as amino, hydroxyl, sulfydryls
Reagent is protected, is widely applied since the advantages that it is active high, reaction condition is mild makes it have, especially in pharmaceutical synthesis
In, as Cefepime, Cefpirome synthesis in.Commercially available Iodotrimethylsilane contains many low-boiling impurity (such as tetramethyls
Base silane and dimethyl diiodo- silane), this impure product is unfavorable for the synthesis of cephalosporin, it is also possible to form medication
Side effect afterwards.The synthetic method of Iodotrimethylsilane has more than 10 kinds at present, more practical at present and be easy to industrialized synthesis side
Method is hexamethyldisiloxane and reacting for iodine and aluminium powder and reacting for hexamethyldisilane and iodine.
A kind of synthetic method of Iodotrimethylsilane is referred in patent CN1962668A, first by aluminium powder, two silicon of hexamethyl
Oxygen alkane and iodine are reacted in a kettle, and distillation obtains Iodotrimethylsilane crude product.Then Iodotrimethylsilane crude product is set
In kettle, copper powder is added, fraction is collected in heating, refined Iodotrimethylsilane is made, 99.0% or more purity, yield is about
66%, yield is extremely low.And iodine and the aluminium triiodide of aluminium solid-solid reaction generation are covered in the surface of iodine and aluminium powder, hinder further
Reaction.
A kind of preparation method of Iodotrimethylsilane is disclosed in patent CN105237559A, it is anhydrous under the protection of nitrogen
Aluminium chloride is warming up to 40-50 DEG C with hexamethyldisiloxane stirring, and 125-140 DEG C of reflux of elemental iodine oil bath is then added portionwise
Reaction 1-1.5 hours, device are changed to distilling apparatus, and air-distillation collects 106-107 DEG C of fraction, obtains Iodotrimethylsilane.Purity
99% or more, yield about 96%.Using in batches plus by the way of iodine in this method, increases the danger of operation and also polluted
Operating environment endangers the health of operating personnel.
A kind of preparation method of Iodotrimethylsilane, (1) hexamethyldisilane input are mentioned in patent CN101230072A
After being stirred and heated to 65-95 DEG C, smart iodine is added portionwise in reaction kettle, and the rear system that iodine adds recycles reaction 5-7 at 100-110 DEG C
Hour.The mass ratio of hexamethyldisilane and smart iodine is 1:1.8-1:1.62；(2) Iodotrimethylsilane to flow back in (1) is thick
In product be added copper powder be back to it is colourless after, distillation obtain Iodotrimethylsilane.The quality of copper powder and raw material hexamethyldisilane it
Than for 0.01-0.02.Yield about 99.8%, content are more than 99%.Deficiency present in the reaction is：Added in batches using high temperature
Iodine, it is not easy to operate while bringing harm to operating personnel；It is higher using hexamethyldisilane cost.
In patent CN102718790A, it is noted that a kind of preparation process of Iodotrimethylsilane：(1) two silicon of hexamethyl is prepared
Alkane：Meta-xylene and metallic potassium are first put into stirred tank, are mixed；Then trim,ethylchlorosilane is added dropwise into stirred tank,
Stop stirring after reaction, material in kettle is imported into washing kettle；(2) it washes：Water is added into washing kettle, after stand it is heavy
Drop, the liquid distillation of generation, solid residue recycling.(3) rectifying：It adds clear liquid into rectifying tower reactor, interval produces hexamethyl two
Silane and middle distillate, then produce meta-xylene；(4) iodine silane synthesizes：The hexamethyldisilane of rectifying output is thrown to reaction
In kettle and iodine is added, Iodotrimethylsilane is generated in 0-0.02Mpa micro-positive pressure systems.Yield is about 94%.It is adopted in this method
With high-risk chemicals metallic potassium, operate dangerous.
The earlier patents CN104926851A of the present inventor is related to a kind of preparation method of Iodotrimethylsilane, with hexamethyl
Disiloxane and iodine are reaction raw materials；Iodine is dissolved in hexamethyldisilane during the reaction, in a manner of dropwise addition into
Row reaction.Ensure that iodine is free from environmental pollution and also do not endanger operating personnel, and reaction speed is fast, high income, the trimethyl iodine silicon of generation
Alkane does not have to refine, and directly distills, and purity is as high as 99.6% or more.
Another earlier patents CN104926850A is related to a kind of preparation method of Iodotrimethylsilane, with two silica of hexamethyl
Alkane, aluminium powder and iodine are reaction raw materials；Iodine is dissolved in hexamethyldisiloxane during the reaction, in a manner of dropwise addition into
Row reaction, the aluminium powder are superfine aluminium power.Research is found using superfine aluminium power reaction speed quickly, and reacts very thorough, reaction
Yield is significantly larger than common aluminium powder；Aluminium powder is thinner, and reaction speed is faster, and yield is higher.Expensive iodine is not excessive in this method, just
Suitable aluminium powder is excessive, and the Iodotrimethylsilane of generation does not have to refine, and directly distills, and purity is as high as 99.3%.
However there are the unsafe problems for adding iodine in batches in the above method；Use dangerous the asking of high-risk chemical metallic sodium potassium
Topic；The various problems such as operating procedure is complicated, not easy to operate, yield is low, the three wastes are more.Research emphasis, which concentrates on, provides a kind of reaction
The preparation process of mild condition, simple for process, safe operation, high income and the few Iodotrimethylsilane of the three wastes.
Invention content
The goal of the invention of the present invention is to solve to exist in the prior art the unsafe problems for adding iodine in batches；Use high-riskization
The unsafe problems of product metallic sodium potassium；The various problems such as operating procedure is complicated, not easy to operate, yield is low, the three wastes are more.This hair
It is bright propose a kind of mild reaction condition, simple for process, safe operation, high income and the few Iodotrimethylsilane of the three wastes system
Standby technique.
The present invention main technical schemes be：Using anhydrous sodium iodide, anhydrous lithium chloride, trim,ethylchlorosilane as raw material,
Iodotrimethylsilane is synthesized in dry nitrogen atmosphere.
The present invention is using following specific technical solution：
A kind of preparation method of Iodotrimethylsilane, includes the following steps：
(1) preparation of anhydrous lithium iodide：Anhydrous sodium iodide, the two molar ratio are added into the organic solvent of anhydrous lithium chloride
It is 1:1-1.1:1, preferably 1.05:1, it is reacted 1-3 hours at 20-60 DEG C；Obtain anhydrous lithium iodide.
(2) preparation of Iodotrimethylsilane：By anhydrous lithium iodide and trim,ethylchlorosilane with molar ratio 1:1-1:3 ratio
Example reacts 8-10h at 20-80 DEG C, and Iodotrimethylsilane is made.
Organic solvent is selected from toluene, hexamethylene, chloroform, dichloromethane, ethyl acetate, acetone, ethyl alcohol in above-mentioned steps (1)
Or mixtures thereof one of.
Further include after completion of the reaction, filtering out the sodium chloride insoluble in organic solvent in above-mentioned steps (1).
The organic solvent recycling steamed in above-mentioned steps (1).
Quaternary ammonium salt catalyst is further added in above-mentioned steps (2), the catalyst can be tetrabutylammonium iodide,
The dosage of catalyst is the 1%-3% of reaction raw materials total weight.
Iodotrimethylsilane finished product is made after rectifying in above-mentioned steps (2), content is more than 99%.
The present invention further comprises recycling for step (3) lithium chloride：Prepare the by-product chlorination of Iodotrimethylsilane
Then lithium, iodate lithium mixture react again with sodium iodide lithium chloride therein being transformed into lithium iodide through dissolving, decoloration, drying
It recycles.
The conversion ratio of the Iodotrimethylsilane of preparation reaches 99%, 99% or more purity.
Specific embodiment：(1) preparation of anhydrous lithium iodide：Anhydrous iodate is added into the organic solvent of anhydrous lithium chloride
Sodium (molar ratio 1:1-1.1:1) latter 20-60 DEG C, is added to react 1-3 hours；After the completion of reaction, filter out insoluble in organic solvent
Sodium chloride, filtrate concentration is dry to obtain lithium iodide, and anhydrous lithium iodide is obtained after dry.The organic solvent recycling steamed.
(2) preparation of Iodotrimethylsilane：Anhydrous lithium iodide and trim,ethylchlorosilane (molar ratio 1:1-1:3) in quaternary ammonium salt catalyst
Or without 80 DEG C of reaction 10h of 20- in the presence of catalyst, Iodotrimethylsilane crude product is made, trimethyl iodine silicon is made after rectifying
Alkane finished product, content are more than 99%.(3) lithium chloride recycles：By-product lithium chloride, the lithium iodide for preparing Iodotrimethylsilane are mixed
Object is closed through dissolving, decoloration, drying, is then reacted again with sodium iodide and lithium chloride therein is transformed into lithium iodide is recycled.
The present invention has the following advantages：
(1) simple for process, it is easy to operate, change traditional hexamethyldisilane, hexamethyldisiloxane prepares iodine silane
Complicated technology.
(2) reaction condition is mild, safe operation, avoids the danger using high-risk chemical metallic potassium, sodium, while also avoiding
High temperature adds iodine problem.
(3) recycling for three kinds of materials is realized during：Prepare the recyclable profit of the organic solvent steamed when lithium iodide
With；Lithium chloride free of losses in entire reaction process, can be recycled；The trimethylchloro-silicane steamed when Iodotrimethylsilane rectifying
Alkane can be applied to lower batch reaction.Recycling for material can reduce production cost.
(4) organic solvent can be toluene, hexamethylene, chloroform, dichloromethane, ethyl acetate, acetone, ethyl alcohol, etc..
(5) catalyst used is quaternary ammonium salt, molecular sieve.
(6) entire production cycle process, output only has Iodotrimethylsilane product and byproduct sodium chloride, without other three wastes
It generates, technique is environmentally protective.
The present invention provides a kind of safe, easily operated Iodotrimethylsilane synthetic routes simple for process.Trimethyl
The conversion ratio of iodine silane can reach 99%, and single batch of yield reaches 94%-97%, apply mechanically rear yield and can reach 99% or more, purity
99% or more.Recycling for three kinds of materials is realized in the process：It is Ke Xunhuanliyong to prepare the organic solvent steamed when lithium iodide；
Lithium chloride free of losses in entire reaction process, can be recycled；The trim,ethylchlorosilane steamed when Iodotrimethylsilane rectifying
Lower batch reaction can be applied to.Recycling for material can reduce production cost.There was only byproduct sodium chloride waste in whole process
Output, it is environmentally safe and disposable.
Description of the drawings
Fig. 1 is the process flow chart of the present invention.
Specific implementation mode
In the following with reference to the drawings and specific embodiments, the present invention is further explained.It should be understood that these embodiments are merely to illustrate
The present invention rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content that the present invention lectures, ability
Field technique personnel can make the present invention various changes or modification, and such equivalent forms also belong to the application appended claims
Book limited range.
Embodiment 1：
Experiment condition：A) anhydrous lithium chloride and anhydrous sodium iodide rate of charge are molar ratio 1:1,60 DEG C of reaction temperature；B) iodine
When silane synthesizes, lithium iodide and trim,ethylchlorosilane rate of charge 1:2,60 DEG C of reaction temperature, catalyst amount 2.5%.
(1) preparation of anhydrous lithium iodide：107.32g iodine is added by several times into the 300ml acetone solns of 30.29g lithium chlorides
Change sodium (molar ratio 1:1) it is reacted 1 hour after, dripping off；After the completion of reaction, sodium chloride is filtered out；Filtrate concentration is evaporated to obtain lithium iodide,
Anhydrous lithium iodide quality 94g (98.04%), yield 96% are obtained after drying.The acetone steamed is recycled, is recycled after water removal.
(2) preparation of Iodotrimethylsilane：By 94g lithium iodides, 154.78g trim,ethylchlorosilanes (molar ratio 1:2) and
2.5% catalyst tetrabutylammonium iodide is in reaction bulb, and under nitrogen atmosphere, certain temperature reacts 10h, and trimethyl iodine silicon is made
Iodotrimethylsilane finished product 136.71g, purity 99.20%, yield 95.48% is made in alkane crude product after rectifying；.
(3) cycling and reutilization of lithium chloride：Prepare the by-product lithium chloride of Iodotrimethylsilane through trim,ethylchlorosilane washing,
Filtering, oven-dried weight 34.5g；Then molten with the acetone after recycling is dry in step (1) according to identical method in step (1)
Solution is added the reaction of 106.13g sodium iodide acetone solns and lithium chloride therein is transformed into lithium iodide, through filtering, concentration, does by several times
92g lithium iodides, content 97.60% are obtained after dry, the rate of recovery 97.4% is recycled.The acetone steamed recycles, after water removal
It recycles.
Embodiment 2：
Experiment condition：Example 1 recycles recycling for lithium iodide and trim,ethylchlorosilane, and other conditions are tested with example 1
Exhibit material, which recycles, can improve Iodotrimethylsilane yield, but on product quality without influence.
(1) preparation of Iodotrimethylsilane：The lithium iodide 92g, 73.58g new three of lithium chloride preparation will be recycled in example 1
Methylchlorosilane, after the washing of trim,ethylchlorosilane fraction and lithium chloride that 77.57g examples one steam trim,ethylchlorosilane mother liquor with
And 2.5% catalyst tetrabutylammonium iodide in reaction bulb, under nitrogen atmosphere, react 10h under certain temperature, be made trimethyl
Iodotrimethylsilane finished product 133.22g, purity 99.32%, yield is made in iodine silane crude product after rectifying：98.56%.
(2) cycling and reutilization of lithium chloride：The by-product lithium chloride 35g for preparing Iodotrimethylsilane, uses trim,ethylchlorosilane
Washing, filtering, drying；Then according to the preparation method of anhydrous lithium iodide, with acetone (the third of one step of example (3) recycling water removal
Ketone) dissolving, the reaction of 99.57g sodium iodide acetone solns is added dropwise, lithium chloride therein is transformed into lithium iodide, through filtering, concentration, does
88.46g lithium iodides, content 98.00% are obtained after dry, the rate of recovery 96.54% is recycled.The acetone steamed is recycled, is removed
It is recycled after water.
Embodiment 3：
Experiment condition：A) anhydrous lithium chloride and anhydrous sodium iodide rate of charge are molar ratio 1.05:1,60 DEG C of reaction temperature；
B) when iodine silane synthesizes, lithium iodide and trim,ethylchlorosilane rate of charge 1:1.2,60 DEG C of reaction temperature, catalyst amount 2.5%.
(1) preparation of anhydrous lithium iodide：151.19g sodium iodides are added by several times into the acetone soln of 44.81g lithium chlorides
(1.05:1) it is reacted 1 hour after, dripping off；After the completion of reaction, sodium chloride is filtered out；Filtrate concentration is evaporated to obtain lithium iodide, after drying
Obtain anhydrous lithium iodide quality 134.12g (97.80%), yield 98%.The acetone steamed is recycled, is recycled after water removal.Nothing
Water lithium chloride and anhydrous sodium iodide rate of charge 1.05:1, lithium iodide conversion ratio increases than example 1.
(2) preparation of Iodotrimethylsilane：By 134.12g lithium iodides, 128.21g trim,ethylchlorosilanes (molar ratio 1:
1.2) and 2.5% catalyst tetrabutylammonium iodide in reaction bulb, under nitrogen atmosphere, certain temperature react 10h, be made three
Iodotrimethylsilane finished product 188.78g, purity 99.51%, yield 95.8% is made in methyl iodide silane crude product after rectifying.Iodate
Lithium and trim,ethylchlorosilane rate of charge 1:When 1.2, product yield is without significantly improving, but content increases.By-product lithium chloride returns
It receives and utilizes.
Embodiment 4：
Experiment condition：A) anhydrous lithium chloride and anhydrous sodium iodide rate of charge are molar ratio 1.05:1,60 DEG C of reaction temperature；
B) when iodine silane synthesizes, lithium iodide and trim,ethylchlorosilane rate of charge 1:1.2, room temperature reaction, catalyst amount 2.5%.
(1) preparation of anhydrous lithium iodide：151.19g sodium iodides are added by several times into the acetone soln of 44.81g lithium chlorides
(1.05:1) it is reacted 1 hour after, dripping off；After the completion of reaction, sodium chloride is filtered out；Filtrate concentration is evaporated to obtain lithium iodide, after drying
Obtain anhydrous lithium iodide quality 134.44g (97.65%), yield 98.08%.The acetone steamed is recycled, is recycled after water removal.
(2) preparation of Iodotrimethylsilane：By 134.44g lithium iodides, 128.31g trim,ethylchlorosilanes (molar ratio 1:
1.2) and 2.5% catalyst tetrabutylammonium iodide in reaction bulb, under nitrogen atmosphere, react 10h at room temperature, be made front three
Iodotrimethylsilane finished product 79.4g, purity 98.86%, yield 40% is made in base iodine silane crude product after rectifying.
Embodiment 5：
Experiment condition：A) anhydrous lithium chloride and anhydrous sodium iodide rate of charge 1.05:1,60 DEG C of reaction temperature；B) iodine silane
When synthesis, lithium iodide and trim,ethylchlorosilane rate of charge 1:1.2,60 DEG C of reactions, do not have to catalyst.(1) system of anhydrous lithium iodide
It is standby：151.19g sodium iodides (1.05 are added by several times into the acetone soln of 44.81g lithium chlorides:1) it is reacted 1 hour after, dripping off；Instead
After the completion of answering, sodium chloride is filtered out；Filtrate concentration is evaporated to obtain lithium iodide, and anhydrous lithium iodide quality 134.80g is obtained after drying
(97.46%), yield 98.15%.The acetone steamed is recycled, is recycled after water removal.
(2) preparation of Iodotrimethylsilane：By 134.80g lithium iodides, 128.42g trim,ethylchlorosilanes (molar ratio 1:
1.2) in reaction bulb, under nitrogen atmosphere, 10h is reacted at 60 DEG C, Iodotrimethylsilane crude product is made, trimethyl is made after rectifying
Iodine silane finished product 179.51g, purity 99.04%, yield 90.53%.
Claims (5)
1. a kind of preparation method of Iodotrimethylsilane, includes the following steps：
(1) preparation of anhydrous lithium iodide：Anhydrous sodium iodide is added into the organic solvent of anhydrous lithium chloride, it is anti-at 20-60 DEG C
It answers 1-3 hours；Obtain anhydrous lithium iodide；
(2) preparation of Iodotrimethylsilane：By anhydrous lithium iodide and trim,ethylchlorosilane with molar ratio 1:1-1:3 ratio exists
60-80 DEG C of reaction 8-10h, is made Iodotrimethylsilane；
Quaternary ammonium salt catalyst is added in above-mentioned steps (2), the dosage of catalyst is the 1%-3% of reaction raw materials total weight.
2. preparation method according to claim 1, it is characterised in that：Organic solvent is selected from toluene, ring in above-mentioned steps (1)
Hexane, chloroform, dichloromethane, ethyl acetate, acetone, or mixtures thereof one of ethyl alcohol.
3. preparation method according to claim 1, it is characterised in that：Further include in above-mentioned steps (1) after completion of the reaction,
Filter out the sodium chloride insoluble in organic solvent.
4. preparation method according to claim 1, it is characterised in that：The organic solvent recycling steamed in above-mentioned steps (1)
It recycles.
5. preparation method according to claim 1, it is characterised in that：The catalyst is tetrabutylammonium iodide.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP3894418A4 (en) * | 2018-12-10 | 2022-08-31 | Entegris, Inc. | Preparation of triiodosilanes |
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| CN109836448A (en) * | 2019-04-08 | 2019-06-04 | 浙江海洲制药有限公司 | A method of preparing Iodotrimethylsilane |
| CN115605432A (en) * | 2020-04-24 | 2023-01-13 | 恩特格里斯公司（Us） | Process for preparing iodosilanes and compositions therefrom |
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| EP3894418A4 (en) * | 2018-12-10 | 2022-08-31 | Entegris, Inc. | Preparation of triiodosilanes |
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Address after: 262725 Shandong city of Weifang province Shouguang Hou town project area nine west 500 meters north of the new road Patentee after: Shandong Boyuan Pharmaceutical Chemical Co., Ltd Address before: 262725 Shandong city of Weifang province Shouguang Hou town project area nine west 500 meters north of the new road Patentee before: SHANDONG BOYUAN PHARMACEUTICAL & CHEMICAL Co.,Ltd. |
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Inventor after: Li Chenglin Inventor after: Zhai Yongli Inventor after: Chu Rongqiang Inventor before: Li Chenglin Inventor before: Wang Qingmin Inventor before: Zhai Yongli Inventor before: Chu Rongqiang |
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Address after: 262725 200m north of the intersection of Xinhai road and Dajiu Road, marine chemical park, Hou Town, Shouguang City, Weifang City, Shandong Province Patentee after: Shandong Boyuan Pharmaceutical Chemical Co.,Ltd. Address before: 262725 Xinsha Road North, 500m west of Dajiu Road, Houzhen project area, Shouguang City, Weifang City, Shandong Province Patentee before: Shandong Boyuan Pharmaceutical Chemical Co.,Ltd. |
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