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1,3-difluoro disiloxane compound manufacturing method

A technology of difluorodisiloxane and manufacturing method, which is applied in the fields of compounds, chemical instruments and methods, organic chemistry, etc. of elements of group 4/14 of the periodic table, and can solve the problem of low yield of alkylchlorosilane compounds and the manufacturing method Unknown and other issues

Inactive Publication Date: 2013-06-05
ADEKA CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As a method for producing 1,3-difluorodisiloxane compounds, a method of reacting 1,3-dichlorodisiloxane compounds with metal fluorides such as antimony trifluoride, copper fluoride, and zinc fluoride is known. method (for example, refer to Patent Document 1, 3), or a method of reacting 1,3-dichlorodisiloxane compound with potassium hydrofluoride (for example, refer to Patent Document 1), but metal fluorides are expensive or toxic There is a problem that the method of reacting potassium hydrofluoride has a problem that the yield of the alkylchlorosilane compound is low
The production methods of known 1,3-difluorodisiloxane compounds in the past all use 1,3-dichlorodisiloxane compounds as raw materials, but 1,3-dichlorodisiloxane compounds need to be prepared from monosilane The production of 1,3-difluorodisiloxane compounds in a one-step reaction from monosilane compounds is unknown

Method used

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  • 1,3-difluoro disiloxane compound manufacturing method

Examples

Experimental program
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Effect test

Embodiment 1

[0035]

[0036] Put 293 g (2 moles) of dimethyldimethoxysilane into a reaction vessel equipped with a stirrer, a thermometer, and a reflux device under a nitrogen atmosphere, stir at 0°C, and simultaneously add 267 g of 15% hydrofluoric acid dropwise over 1 hour (2.2 mol as hydrogen fluoride), after the dropwise addition, stirring was further continued at 0° C. for 30 minutes. Then, the temperature was raised to 60° C. over 30 minutes, and further stirred at 60° C. for 60 minutes. 48 g of dibutyl ether was put into the reaction vessel, stirred and left to stand, the water layer was removed, the remaining organic layer was transferred to a separatory funnel and washed with 60 ml of saturated brine, and then the organic layer was dried over anhydrous sodium sulfate. The organic layer was distilled off to obtain 119 g of 1,3-difluoro-1,1,3,3-tetramethyldisiloxane (70% yield).

Embodiment 2

[0038]

[0039] In the same reaction vessel as in Example 1, under a nitrogen atmosphere, 182.5 g (1 mole) of 3-chloropropylmethyldimethoxysilane and 120 g of methanol were added, stirred at 0°C, and dropped over 1 hour. After adding 65 g of 46% hydrofluoric acid (1.2 mol as hydrogen fluoride) dropwise, stirring was further continued at 0° C. for 30 minutes. Then, the temperature was raised to 60° C. over 30 minutes, and further stirred at 60° C. for 60 minutes. 150 g of hexane and 150 g of saturated brine were put into the reaction vessel, stirred and left to stand, the water layer was removed, the remaining organic layer was transferred to a separatory funnel and washed with 60 g of saturated aqueous sodium bicarbonate solution, and then the organic layer was washed with water and sodium sulfate to dry. The organic layer was distilled off to obtain 121 g of 1,3-bis(3-chloropropyl)-1,3-difluoro-1,3-dimethyldisiloxane (82% yield).

Embodiment 3

[0041]

[0042] In the same reaction vessel as in Example 1, under a nitrogen atmosphere, 182.5 g (1 mole) of phenylmethyldimethoxysilane and 120 g of methanol were added, stirred at 0°C, and 23% After adding 130 g of hydrofluoric acid (1.2 mol as hydrogen fluoride) dropwise, stirring was further continued at 0° C. for 30 minutes. Then, the temperature was raised to 60° C. over 30 minutes, and further stirred at 60° C. for 60 minutes. 150 g of hexane and 150 g of saturated brine were put into the reaction vessel, stirred and left to stand, the water layer was removed, the remaining organic layer was transferred to a separatory funnel and washed with 60 g of saturated aqueous sodium bicarbonate solution, and then the organic layer was washed with water and sodium sulfate to dry. The organic layer was distilled off to obtain 106 g of 1,3-difluoro-1,3-diphenyl-1,3-dimethyldisiloxane (72% yield).

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Abstract

A 1,3-difluoro disiloxane compound manufacturing method indicated by the following formula (2) is characterized in that the disiloxane compound is reacted with hydrofluoric acid. (in the formula, R1 and R2 respectively and independently indicates an alkyl which is 1 to 8 in carbon atom number, an alkenyl which is 2 to 8 in carbon atom number, an aralkyl which is 7 to 8 in carbon atom number, and a halogenate which is 1 to 8 in carbon atom number).

Description

technical field [0001] The present invention relates to a method for producing 1,3-difluorodisiloxane compounds. Background technique [0002] 1,3-Difluorodisiloxane compound has moderate reactivity, excellent stability, and does not contain chlorine or bromine, which cause metal corrosion, so it is used as a raw material for the production of silicon-based polymer films (for example, refer to Patent Documents 1 and 2), electrolyte solution additives for non-aqueous electrolyte secondary batteries (for example, refer to Patent Document 3), and the like are useful. As a method for producing 1,3-difluorodisiloxane compounds, a method of reacting 1,3-dichlorodisiloxane compounds with metal fluorides such as antimony trifluoride, copper fluoride, and zinc fluoride is known. method (for example, refer to Patent Document 1, 3), or a method of reacting 1,3-dichlorodisiloxane compound with potassium hydrofluoride (for example, refer to Patent Document 1), but metal fluorides are ex...

Claims

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Application Information

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IPC IPC(8): C07F7/12H01M10/0567H01B3/18
CPCY02E60/12Y02E60/10
Inventor 泷敬之渡边裕知涩谷厚辉田崎晃子
Owner ADEKA CORP
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