M-methylphenyldiethoxymethylsilane and preparation method thereof

A technology of m-methylphenyldiethoxymethylsilane and methylphenyldiethoxymethylsilane, which is applied to compounds containing silicon element m-methylphenyldiethoxymethylsilane and its In the field of synthesis, it can solve the problems of solvent recycling and environmental pollution, and achieve the effects of saving operating costs, simple separation and purification, and improving the utilization rate of reaction equipment

Active Publication Date: 2013-01-30
HANGZHOU NORMAL UNIVERSITY
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  • Abstract
  • Description
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Benefits of technology

This patented technology reduces harmful emissions from chemical reactions involving tetrafluorobenzene (TFB). It uses less expensive or environmentally friendly substances like TFB instead of chloroform gas. By doing this, it simplifies the manufacturing processes while also reducing waste generated during disposal operations. Additionally, there're benefits that include improved efficiency and reduced cost associated with separating pure products produced through conventional methods such as distillations. Overall, these technical improvements improve overall performance and reduce negative impact on our planet's ecosystems

Problems solved by technology

The patent text discusses the synthesis of a compound called meta-substituted methylphenyldiethoxymethylsilane, which is used to make silicone products with high refractive index. The current method of synthesis, called the sodium condensation method, requires the use of a large amount of solvent, such as toluene, which can cause environmental pollution and difficulties in solvent recycling. The technical problem addressed in the patent is to find a more environmentally friendly and efficient method for synthesizing meta-substituted methylphenyldiethoxymethylsilane.

Method used

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  • M-methylphenyldiethoxymethylsilane and preparation method thereof

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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 100g (0.561 moles) of methyltriethoxysilane, and add 18g (0.783 moles) of freshly cut Sodium flakes, heat up to 102°C, beat the sodium flakes into sodium sand; within 4 hours, add 47g (0.371 moles) m-chlorotoluene into the reaction system dropwise through a constant pressure dropping funnel, and control the reaction temperature between 108~110 ℃, continue to react for 2 h 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 cool at 25°C Keep it for 1h; then add 10mL (0.083 moles) of dimethyldichlorosilane dropwise to the mixture within 1h to neutralize the generated sodium alkoxide; after the dropwise addition, continue the reaction at this temperature for 3h. Then the reaction mixture was suction-filtered under reduced pressure to obtain a...

Embodiment 2

[0026] In a dry 1000mL four-neck flask equipped with a reflux condenser, a mechanical stirrer and a Pt-100 platinum resistance, add 450g (2.524 moles) of methyltriethoxysilane, and add 58.2g (2.530 moles) of freshly chopped The sodium flakes were heated up to 105°C, and the sodium flakes were beaten into sodium sand; within 2 hours, 160g (1.264 moles) of m-chlorotoluene was added dropwise to the reaction system through a constant pressure dropping funnel, and the reaction temperature was controlled between 102~ 105°C, continue to react for 4 hours after the dropwise addition, after cooling to 30°C, slowly add 5.1g (0.111 moles) of absolute ethanol within 1.0h to neutralize the excess metallic sodium, and then cool at 30°C Then, 30mL (0.257 moles) of methyltrichlorosilane was added dropwise to the mixture within 2h to neutralize the generated sodium alkoxide; after the dropwise addition was completed, the reaction was continued at this temperature for 4h. Then the reaction mixt...

Embodiment 3

[0029]In a dry 500mL four-neck flask equipped with a reflux condenser, a mechanical stirrer and a Pt-100 platinum resistance, add 253g (1.419 moles) of methyltriethoxysilane, and add 21.8g (0.948 moles) of freshly chopped The sodium flakes were heated up to 104 ° C, and the sodium flakes were beaten into sodium sand; within 6 hours, 60 g (0.474 moles) of m-chlorotoluene was added dropwise to the reaction system through a constant pressure dropping funnel, and the reaction temperature was controlled between 105~ 108°C, continue to react for 5 hours after the dropwise addition, after cooling to 20°C, slowly add 2.0g (0.043 moles) of absolute ethanol within 1.0h to neutralize the excess metal sodium, and then cool at 20°C Then, 13mL (0.108 moles) of dimethyldichlorosilane was added dropwise to the mixture within 1.5h to neutralize the generated sodium alkoxide; after the dropwise addition, the reaction was continued at this temperature for 2h. Then the reaction mixture was suctio...

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Abstract

The invention relates to the field of organic silicon chemistry and discloses an m-methylphenyldiethoxymethylsilane and a preparation method thereof. The preparation method solves the problem that in the existing sodium condensation method-based synthesis of m-methylphenyldiethoxymethylsilane, a large amount of a solvent is used and thus environmental pollution is caused and solvent recycle is difficult. The m-methylphenyldiethoxymethylsilane is synthesized from methyltriethoxysilane and m-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

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Claims

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Application Information

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Owner HANGZHOU NORMAL UNIVERSITY
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