CN1962668A - Process for synthesizing iodotrimethylsilane - Google Patents
Process for synthesizing iodotrimethylsilane Download PDFInfo
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- CN1962668A CN1962668A CN 200610097774 CN200610097774A CN1962668A CN 1962668 A CN1962668 A CN 1962668A CN 200610097774 CN200610097774 CN 200610097774 CN 200610097774 A CN200610097774 A CN 200610097774A CN 1962668 A CN1962668 A CN 1962668A
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- iodotrimethylsilane
- iodine
- synthetic method
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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
The present invention relates to a kind of synthetic method of Chemicals.
Background technology
Usually; Iodotrimethylsilane can with contain easily the dissociate organosilicon reagent of derivative of hydroxyl, carboxyl and amino compound formation; these reagent are commonly used to protect hydroxyl in organic synthesis, the application of Iodotrimethylsilane is very wide, plays important effect in organic reaction.The demand that Western medicine ceftazime intermediate is produced in the conduct of Iodotrimethylsilane increases year by year.The producer of domestic batch process trimethylammonium iodine silicon does not almost have, the Iodotrimethylsilane of all circulations or be a small amount of of domestic each Laboratory Production, or from external import.
Surplus the synthetic method of Iodotrimethylsilane has ten more than the kind, practical and be easy to the reaction that industrialized synthetic method is hexamethyldisiloxane, iodine and aluminium powder and hexamethyldisilane and iodine.Because these two kinds of method raw materials are easy to get, technology is simple, the productive rate height.But the Iodotrimethylsilane that has just formed at present sale is in process of production owing to adopt single stage method synthetic, also contain a lot of lower boiling impurity (tetramethylsilane and dimethyl diiodo-silane) through nucleus n-ness spectrum proof the inside, thisly contain assorted product and be unfavorable for the synthetic of ceftazime, also might form the side effect after the medication.
Summary of the invention
The object of the invention is to invent the synthetic method of the high Iodotrimethylsilane of a kind of product purity.
The present invention reacts aluminium powder, hexamethyldisiloxane and iodine earlier in reactor, distillation obtains the Iodotrimethylsilane crude product, then, again the Iodotrimethylsilane crude product is placed in the still kettle, add copper powder, heat up, collect cut, make the purified Iodotrimethylsilane.
The present invention through special technology, makes purity up to the Iodotrimethylsilane elaboration more than 99.0% with the Iodotrimethylsilane crude product, has made things convenient for the processing of back road, can be beneficial to the side effect that reduces and reduce the ceftazime Western medicine.
In the present invention, the weight ratio of the copper powder of adding and Iodotrimethylsilane crude product is 1: 50～70.
By above suitable feed ratio, can reduce the decomposition of Iodotrimethylsilane.
In addition, when synthetic Iodotrimethylsilane crude product, the molar ratio of aluminium powder, hexamethyldisiloxane and iodine is: 1～2: 1: 1.5～1.6.
Usually the feed ratio of iodine and hexamethyldisiloxane is 2: 1, has caused a large amount of wastes of iodine, is unfavorable for the reduction of production cost.
Among the present invention, the concrete grammar of producing the Iodotrimethylsilane crude product is: earlier aluminium powder and hexamethyldisiloxane are dropped into reactor, stir, add iodine after material in the still is warmed up to 55～65 ℃, after question response causes, temperature of charge is 65～75 ℃ in the control still, is warmed up to 140 ± 10 ℃ more gradually, back flow reaction 1.5～2h, change water distilling apparatus into, 100～150 ℃ of cuts are collected in air distillation, obtain the Iodotrimethylsilane crude product.
In order to reduce the usage quantity of production process iodine, the present invention also after producing the Iodotrimethylsilane crude product, reclaims iodine from the reactor surplus solution.
The method that reclaims iodine is: after stopping distillation, solution in the reactor is cooled to 140 ± 10 ℃, add the high boiling hydrocarbon kind solvent, cool to 60～70 ℃ again, adjusting the solution pH value is 6, filters, and removes Al (OH)
3Solid; With the filtrate layering, add H again at lower floor's aqueous phase
2SO
4, adjusting pH value is 1～2, and keeps this pH value, drips 30% hydrogen peroxide, separates out thick iodine.
Above-mentioned high boiling hydrocarbon kind solvent can be dimethylbenzene or paraffin oil.
Also thick iodine can be placed in the container, add dense H
2SO
4, be warmed up to 130～140 ℃, iodine is all melted, while hot iodine is emitted, solidify, pulverize, further obtain pure iodine, be beneficial to circularly iodine is used for produce.
Among the present invention, when producing the Iodotrimethylsilane crude product, the residual high boiling material when front-end volatiles when also input is made with extra care Iodotrimethylsilane in reactor and refining Iodotrimethylsilane in the still kettle.
High boiling material recycles during with front-end volatiles and refining Iodotrimethylsilane, can improve the yield of Iodotrimethylsilane.
Embodiment
Operation steps:
1, produce the Iodotrimethylsilane crude product:
In the exsiccant reactor, add aluminium powder 13.5kg (500mol), hexamethyldisiloxane 64.8kg (400mol), start stirrer, the oil bath heating, make the interior material of still be warmed up to 55～65 ℃, begin to add iodine, after question response causes, controlled temperature is at 65～75 ℃, in 1h, slowly add smart iodine 157.5kg (620mol) in batches, be warmed up to 140 ± 10 ℃ gradually, back flow reaction 1.5～2h, change water distilling apparatus into, 100～150 ℃ of cuts are collected in air distillation, obtain Iodotrimethylsilane crude product 134.8kg (84.25%).
Temperature in the kettle stops distillation at 210～220 ℃, cools to 140 ± 10 ℃, adds 100L high boiling hydrocarbon kind solvent (as dimethylbenzene or paraffin wet goods), cools to 60～70 ℃, adds 20% KOH solution 400kg, adds, and measures and adjust solution PH=6.Filter, remove Al (OH)
3Solid, the filtrate layering adds H to lower floor's aqueous phase
2SO
4, adjust PH=1～2, be controlled at PH=1～2 then, the hydrogen peroxide of dropping 30% is 31kg altogether, iodine is separated out fully, the thick iodine 73.4kg of filtered and recycled, content 95.1% (97.2%).
The thick iodine of hydrous powdery shape that reclaims is added in another reactor, add 98% dense H
2SO
4, be warmed up to 130～140 ℃, iodine is all melted, while hot iodine is emitted, solidify, pulverize, obtain the iodine 68.5kg (rate of recovery 98.16%) of content 〉=99.5%, total yield is 95.4%.
2, produce the Iodotrimethylsilane elaboration:
134.8kg Iodotrimethylsilane crude product is joined in the still kettle, add about 2kg copper powder simultaneously, heat temperature raising distills.Collect 24～104 ℃ of cut 6.9kg (5.12%), 104～106 ℃ of cuts are finished product 105.8kg (yield 78.49%), and residual high boiling material is 16.0kg in the still.
Through above method, obtain that 105.8kg water white transparency corrodibility flammable liquid---Iodotrimethylsilane elaboration, purity are 99.26%.
3, the Iodotrimethylsilane crude product is produced in recirculation:
Aluminium powder, hexamethyldisiloxane and iodine are reacted in reactor
In the exsiccant reactor, add aluminium powder 16.2kg (600mol), hexamethyldisiloxane 64.8kg (400mol), front-end volatiles (Iodotrimethylsilane crude product) 6.9kg, high boiling material 16.0kg, start stirrer, the oil bath heating, make the interior material of still be warmed up to 55～65 ℃, begin to add iodine, after question response causes, controlled temperature slowly adds smart iodine 163.3kg (643mol) at 65～75 ℃ in batches in 1h, be warmed up to 140 ± 10 ℃ gradually, back flow reaction 1.5～2h, change water distilling apparatus into, 100～150 ℃ of cuts are collected in air distillation, obtain Iodotrimethylsilane crude product 145.7kg, (yield 91.06%).
The recycling of iodine is the same.Iodotrimethylsilane crude product 145.7kg, by obtaining 123.2kg Iodotrimethylsilane elaboration after the rectifying, content 99.31%, yield are 84.56%.
Claims (9)
1, a kind of synthetic method of Iodotrimethylsilane, earlier aluminium powder, hexamethyldisiloxane and iodine are reacted in reactor, distillation, obtain the Iodotrimethylsilane crude product, it is characterized in that the Iodotrimethylsilane crude product is placed in the still kettle, add copper powder, heat up, collect cut, be the purified Iodotrimethylsilane.
2,, it is characterized in that the copper powder that adds and the weight ratio of Iodotrimethylsilane crude product are 1: 50～70 according to a kind of synthetic method of the described Iodotrimethylsilane of claim 1.
3, according to a kind of synthetic method of the described Iodotrimethylsilane of claim 1, when it is characterized in that synthesizing the Iodotrimethylsilane crude product, the molar ratio of aluminium powder, hexamethyldisiloxane and iodine is: 1～2: 1: 1.5～1.6.
4, according to a kind of synthetic method of the described Iodotrimethylsilane of claim 3, it is characterized in that earlier aluminium powder and hexamethyldisiloxane being dropped into reactor, stir, add iodine after material in the still is warmed up to 55～65 ℃, after question response causes, temperature of charge is 65～75 ℃ in the control still, is warmed up to 140 ± 10 ℃ more gradually, back flow reaction 1.5～2h, change water distilling apparatus into, 100～150 ℃ of cuts are collected in air distillation, obtain the Iodotrimethylsilane crude product.
5,, it is characterized in that after producing the Iodotrimethylsilane crude product, from the reactor surplus solution, reclaiming iodine according to a kind of synthetic method of claim 1 or 2 or 3 or 4 described Iodotrimethylsilanes.
6,, after it is characterized in that stopping to distill, solution in the reactor is cooled to 140 ± 10 ℃ according to a kind of synthetic method of the described Iodotrimethylsilane of claim 5, add the high boiling hydrocarbon kind solvent, cool to 60～70 ℃ again, adjusting the solution pH value is 6, filter, remove Al (OH)
3Solid; With the filtrate layering, add H again at lower floor's aqueous phase
2SO
4, adjusting pH value is 1～2, and keeps this pH value, drips 30% hydrogen peroxide, separates out thick iodine.
7,, it is characterized in that described high boiling hydrocarbon kind solvent is dimethylbenzene or paraffin oil according to a kind of synthetic method of the described Iodotrimethylsilane of claim 6.
8, according to a kind of synthetic method of the described Iodotrimethylsilane of claim 6, it is characterized in that thick iodine is placed in the container, add dense H
2SO
4, be warmed up to 130～140 ℃, iodine is all melted, while hot iodine is emitted, solidify, pulverize, obtain pure iodine.
9, according to a kind of synthetic method of the described Iodotrimethylsilane of claim 4, when it is characterized in that producing the Iodotrimethylsilane crude product, the residual high boiling material when front-end volatiles when also input is made with extra care Iodotrimethylsilane in reactor and refining Iodotrimethylsilane in the still kettle.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100977746A CN100560590C (en) | 2006-11-27 | 2006-11-27 | A kind of synthetic method of Iodotrimethylsilane |
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| CNB2006100977746A CN100560590C (en) | 2006-11-27 | 2006-11-27 | A kind of synthetic method of Iodotrimethylsilane |
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| Publication Number | Publication Date |
|---|---|
| CN1962668A true CN1962668A (en) | 2007-05-16 |
| CN100560590C CN100560590C (en) | 2009-11-18 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100564384C (en) * | 2008-02-04 | 2009-12-02 | 吴江信谊化工有限公司 | Preparation method of iodotrimethylsilane |
| CN102718790A (en) * | 2012-06-08 | 2012-10-10 | 新亚强硅化学江苏有限公司 | Preparation process of trimethyl idodine silicon hydride |
| CN104926850A (en) * | 2015-07-17 | 2015-09-23 | 山东博苑医药化学有限公司 | Iodotrimethylsilane preparation method |
| CN104945398A (en) * | 2014-03-26 | 2015-09-30 | 南京优科生物医药研究有限公司 | Method for preparing Moxifloxacin impurity E |
| CN104961759A (en) * | 2015-06-25 | 2015-10-07 | 浙江海洲制药有限公司 | Trimethyl halogenosilane preparation method |
| CN108299492A (en) * | 2018-03-15 | 2018-07-20 | 河北百灵威超精细材料有限公司 | A kind of purification process of organo-silicon compound |
-
2006
- 2006-11-27 CN CNB2006100977746A patent/CN100560590C/en active Active
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100564384C (en) * | 2008-02-04 | 2009-12-02 | 吴江信谊化工有限公司 | Preparation method of iodotrimethylsilane |
| CN102718790A (en) * | 2012-06-08 | 2012-10-10 | 新亚强硅化学江苏有限公司 | Preparation process of trimethyl idodine silicon hydride |
| CN104945398A (en) * | 2014-03-26 | 2015-09-30 | 南京优科生物医药研究有限公司 | Method for preparing Moxifloxacin impurity E |
| CN104945398B (en) * | 2014-03-26 | 2017-10-20 | 南京优科生物医药研究有限公司 | A kind of moxifloxacin impurity E preparation method |
| CN104961759A (en) * | 2015-06-25 | 2015-10-07 | 浙江海洲制药有限公司 | Trimethyl halogenosilane preparation method |
| CN104961759B (en) * | 2015-06-25 | 2017-10-27 | 浙江海洲制药有限公司 | A kind of preparation method of trimethyl halosilanes |
| CN104926850A (en) * | 2015-07-17 | 2015-09-23 | 山东博苑医药化学有限公司 | Iodotrimethylsilane preparation method |
| CN108299492A (en) * | 2018-03-15 | 2018-07-20 | 河北百灵威超精细材料有限公司 | A kind of purification process of organo-silicon compound |
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| Publication number | Publication date |
|---|---|
| CN100560590C (en) | 2009-11-18 |
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