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P-benzyldiethoxymethylsilane and preparation method thereof

A technology of benzyldiethoxymethylsilane and methyltriethoxysilane, which is applied in the field of silicon-containing compound p-benzyldiethoxymethylsilane and its synthesis, and can solve solvent recovery Utilization, solvent environmental pollution and other problems, to achieve the effect of saving operating costs, simple separation and purification, and improving conversion rate

Active Publication Date: 2013-01-30
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • 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 para-substituted benzyldiethoxymethylsilane by sodium condensation method, the present invention proposes a p-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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  • P-benzyldiethoxymethylsilane and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0024] In a dry 250mL four-neck flask equipped with a reflux condenser, a mechanical stirrer and a Pt-100 platinum resistance, add 82g (0.4599 moles) of methyltriethoxysilane, and add 10.54g (0.4585 moles) of freshly chopped The sodium flakes were heated up to 110°C, and the sodium flakes were beaten into sodium sand; within 2 hours, 29.2g (0.2307 moles) of p-chlorotoluene was added dropwise to the reaction system through a constant pressure dropping funnel, and the reaction temperature was controlled between 108 ~112°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 wait for 25 Maintain at ℃ 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 m...

Embodiment 2

[0027] In a dry 250mL four-necked flask equipped with a reflux condenser, a mechanical stirrer and a Pt-100 platinum resistance, add 122.4g (0.6865 moles) of methyltriethoxysilane, and add 10.9g (0.4741 moles) of new Cut the sodium flakes, raise the temperature to 110°C, and beat the sodium flakes into sodium sand; within 1 hour, add 29.2g (0.2307 moles) of p-chlorotoluene into the reaction system dropwise through a constant pressure dropping funnel, and control the reaction temperature between 108~112°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 metal 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 ...

Embodiment 3

[0030] In a dry 250mL four-necked flask equipped with a reflux condenser, a mechanical stirrer and a Pt-100 platinum resistance, add 163.2g (0.9153 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 2 hours, add 29.2g (0.2307 moles) of p-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 filtered under reduce...

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Abstract

The invention relates to the field of organic chemistry and provides p-benzyldiethoxymethylsilane and a preparation method thereof. The preparation method solves the problem that in sodium condensation method-based synthesis of p-substituted benzyldiethoxymethylsilane, a large amount of a solvent is used so that environmental pollution is produced and solvent recycle is difficult. The preparation method comprises that the p-benzyldiethoxymethylsilane is synthesized from methyl triethoxysilane and p-chlorotoluene as raw materials by a sodium condensation method. The preparation method does not use 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 p-benzyldiethoxymethylsilane and a synthesis method thereof. Background technique [0002] Para-substituted benzyldiethoxymethylsilane (p-benzyldiethoxymethylsilane) is an important synthetic monomer, which is relatively active 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 p-substituted benzyldiethoxymethylsilane by sodium condensation method is still in its infancy. The sodium condensation method is a classic method for constructing organosilicon compounds at present, that is, t...

Claims

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Application Information

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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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