O-benzyldiethoxymethylsilane and preparation method thereof

A technology of o-benzyldiethoxymethylsilane and benzyldiethoxymethylsilane, applied in chemical instruments and methods, compounds of elements of Group 4/14 of the periodic table, organic chemistry, etc., It can solve the problems of solvent environmental pollution and solvent recycling, and achieve the effect of simple separation and purification, saving operating costs and simple process.

Active Publication Date: 2013-01-30
HANGZHOU NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the problem of environmental pollution and solvent recycling when using a large amount of solvent to synthesize ortho-substituted benzyldiethoxymethylsilane by sodium condensation method, the present invention proposes a kind of ortho-benzyldiethoxymethylsilane A base silane and a synthetic method thereof, the method does not use solvents such as toluene, the reaction conditions are mild, and the process is simple; it is very suitable for large-scale industrial production

Method used

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  • O-benzyldiethoxymethylsilane and preparation method thereof

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Experimental program
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Embodiment 1

[0023] In a dry 250mL four-neck flask equipped with a reflux condenser, a mechanical stirrer and a Pt-100 platinum resistance, add 163.4g (0.9214 moles) of methyltriethoxysilane, and add 10.8g (0.4698 moles) of new Cut the sodium flakes, raise the temperature to 103°C, and beat the sodium flakes into sodium sand; within 1 hour, add 29.2g (0.2307 moles) of o-chlorotoluene into the reaction system dropwise through a constant pressure dropping funnel, and control the reaction temperature between 102~104°C, continue to react for 2 hours after the dropwise addition, after cooling to 25°C, slowly add 1.5g (0.0326 moles) of absolute ethanol within 0.5h to neutralize the excess metal sodium, and then add Maintain at 25°C for 1 h; then add 9.4 mL (0.0805 mol) of methyltrichlorosilane dropwise to the mixture within 1 h to neutralize the generated sodium alkoxide; after the addition is complete, continue the reaction at this temperature for 3 h. Then the reaction mixture was suction-filt...

Embodiment 2

[0026] In a dry 250mL four-neck flask equipped with a reflux condenser, a mechanical stirrer and a Pt-100 platinum resistance, add 163.8g (0.9187 moles) of methyltriethoxysilane, and add 10.6g (0.4611 moles) of new Cut the sodium flakes, raise the temperature to 95°C, and beat the sodium flakes into sodium sand; within 2 hours, add 29.2g (0.2307 moles) of o-chlorotoluene dropwise into the reaction system through a constant pressure dropping funnel, and control the reaction temperature between 95~98°C, continue to react for 4 hours after the dropwise addition, after cooling to 30°C, slowly add 3.1g (0.0673 moles) of absolute ethanol within 1.0h to neutralize the excess metallic sodium, and then add Maintain at 30°C for 1.5h; then add 9.4mL (0.0805mol) methyltrichlorosilane dropwise to the mixture within 2h to neutralize the generated sodium alkoxide; after the dropwise addition, continue the reaction at this temperature for 4h . Then the reaction mixture was suction-filtered u...

Embodiment 3

[0029] In a dry 250mL four-necked flask equipped with a reflux condenser, a mechanical stirrer and a Pt-100 platinum resistance, add 81.9g (0.4593 moles) of methyltriethoxysilane, and add 10.8g (0.4698 moles) of new Cut the sodium flakes, raise the temperature to 95°C, and beat the sodium flakes into sodium sand; within 6 hours, add 29.2g (0.2307 moles) of o-chlorotoluene into the reaction system dropwise through a constant pressure dropping funnel, and control the reaction temperature between 95~98°C, continue to react for 5 hours after the dropwise addition, after cooling to 20°C, slowly add 5.0g (0.1085 moles) of absolute ethanol within 1.0h to neutralize the excess metal sodium, and then add Maintain at 20°C for 1.5h; then add 16.0mL (0.1327mol) dimethyldichlorosilane dropwise to the mixture within 1.5h to neutralize the generated sodium alkoxide; after the addition is complete, continue at this temperature Reaction 2h. Then the reaction mixture was suction-filtered under...

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Abstract

The invention relates to the field of organic silicon chemistry and provides o-benzyldiethoxymethylsilane and a preparation method thereof. The preparation method solves the problem that in the existing sodium condensation method-based synthesis of o-substituted benzyldiethoxymethylsilane, a large amount of a solvent is used so that environmental pollution is caused and solvent recycle is difficult. The o-benzyldiethoxymethylsilane is synthesized from methyltriethoxysilane and o-chlorotoluene as raw materials by a sodium condensation method. The preparation method does not adopt a toluene solvent, allows mild reaction conditions, has simple processes and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the field of organic chemistry, in particular to a silicon-containing compound o-benzyldiethoxymethylsilane and a synthesis method thereof. Background technique [0002] Ortho-substituted benzyldiethoxymethylsilane (ortho-benzyldiethoxymethylsilane) is an important synthetic monomer, which is relatively active in nature and can be used to synthesize organosilicon intermediates and Polymer compounds such as silicone oil and silicone rubber, because of their high molar refractive index, can be used to increase the refractive index of silicone materials, and have important uses in the fields of LED packaging, optical waveguide devices, optical interconnect devices, and optical lenses. [0003] At present, the research on the synthesis of ortho-substituted benzyldiethoxymethylsilane by sodium condensation method is still in its infancy. The sodium condensation method is a classic method for constructing organosilicon compounds at ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 伍川曹健董红蒋剑雄武侠程大海
Owner HANGZHOU NORMAL UNIVERSITY
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