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Production process of trimethylsilylacetylene

A technology of trimethylsilyl acetylene and production process, applied in the direction of silicon organic compounds and the like, can solve the problems of harsh production conditions, difficult to obtain raw materials, complicated production process, etc., and achieves low production cost, high product quality, and high yield. Effect

Inactive Publication Date: 2014-07-02
ANQING FENGYUAN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the raw materials used in the synthesis method of trimethylsilylacetylene are generally difficult to obtain, the price is high, the production process is relatively complicated, the production conditions are harsh, and the yield is low.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A production process for trimethylsilylacetylene, comprising the following steps: wherein the raw materials used are metal magnesium, vinyl chloride, tetrahydrofuran, cuprous halide, 1,2-dibromoethane, trimethylchlorosilane and water in molar ratios respectively For: 1:1.5:13:0.15:0.07:0.04:2.5:130.

[0022] (1) Add the measured tetrahydrofuran and metal magnesium into the reaction kettle, then add iodine and 1,2-dibromoethane, raise the temperature to 60°C, feed the measured amount of vinyl chloride, keep the temperature for 3 hours, and cool down to 20°C. Add the metered cuprous halide, stir, start to add the metered mixture of tetrahydrofuran and trimethylchlorosilane, raise the temperature to 50°C, and keep it warm for 5 hours; then distill the generated vinyltrimethylsilane, good water for washing;

[0023] (2) Dissolve the vinyltrimethylsilane prepared in step (1) in methanol, control the temperature at 20°C, add an equal amount of bromine dropwise, until the rea...

Embodiment 2

[0025] A production process for trimethylsilylacetylene, comprising the following steps: wherein the raw materials used are metal magnesium, vinyl chloride, tetrahydrofuran, cuprous halide, 1,2-dibromoethane, trimethylchlorosilane and water in molar ratios respectively It is: 1:1:10:0.1:0.06:0.03:2:100.

[0026] (1) Add the measured tetrahydrofuran and metal magnesium into the reaction kettle, then add iodine and 1,2-dibromoethane, raise the temperature to 60°C, feed the measured amount of vinyl chloride, keep the temperature for 3 hours, and cool down to 30°C. Add the metered cuprous halide, stir, start to add the metered mixture of tetrahydrofuran and trimethylchlorosilane, raise the temperature to 60°C, and keep it warm for 5 hours; then distill the generated vinyl trimethylsilane, good water for washing;

[0027] (2) Dissolve the vinyltrimethylsilane prepared in step (1) in methanol, control the temperature at 15°C, add an equal amount of bromine dropwise, and then slowly...

Embodiment 3

[0029] A production process of trimethylsilylacetylene, which comprises the following steps: wherein the raw materials used are metal magnesium, vinyl chloride, tetrahydrofuran, cuprous halide, 1,2-dibromoethane, trimethylchlorosilane and water mole The ratios are: 1:2:15:0.2:0.08:0.05:3:150.

[0030] (1) Add the measured tetrahydrofuran and metal magnesium into the reaction kettle, then add iodine and 1,2-dibromoethane, raise the temperature to 60°C, feed the measured amount of vinyl chloride, keep the temperature for 3 hours, and cool down to 30°C. Add the metered cuprous halide, stir, start to add the metered mixture of tetrahydrofuran and trimethylchlorosilane, raise the temperature to 60°C, and keep it warm for 5 hours; then distill the generated vinyl trimethylsilane, good water for washing;

[0031] (2) Dissolve the vinyltrimethylsilane prepared in step (1) in methanol, control the temperature at 20°C, add an equal amount of bromine dropwise, and then slowly add an equ...

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PUM

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Abstract

The invention discloses a production process of trimethylsilylacetylene, comprises the following steps: (1) adding the measured tetrahydrofuran and magnesium metal into a reaction still, adding iodine and 1,2-dibromoethane, warming to 50-60 DEG.C, introducing the measured chloroethylene, heat-insulating for 3 hours, cooling to 20-30 DEG.C, adding a catalyst, stirring, and then adding the measured mixed solution of tetrahydrofuran and trimethylchlorosilane, warming to 50-60 DEG.C, heat-insulating for 5 hours; distilling the produced vinyl trimethylsilyl to be dissolved in methanol, controlling temperature at 15-20 DEG.C, dropwise adding equal bromine, reacting until floor fading, slowly dropwise adding equal alkaline methanol solution, controlling temperature at 30-40 DEG.C, reacting HPLC monitoring until the reaction is finished, adding dichloromethane, filtering to remove salt, and concentrating to obtain a finished product. The raw materials adopted by the invention are available and low in price, the production cost is low, the product quality is high, the reaction condition is mild, the yield is high, and the production process is capable of producing the trimethylsilylacetylene on large scale.

Description

technical field [0001] The invention relates to the technical field of compound synthesis, in particular to a production process of trimethylsilylacetylene. Background technique [0002] Trimethylsilylacetylene is an important spice and pharmaceutical intermediate, one of the important silicon-based chemical raw materials, and an important alkynylation reagent, which is essential in the preparation of various mono-alkyne and polyalkyne Few synthetic primitives. In addition, there are many applications in heterocyclic chemistry, carbon-carbon coupling, drug synthesis, catalytic chemistry, and materials industry. At present, the raw materials used in the synthesis method of trimethylsilylacetylene are generally difficult to obtain, the price is high, the production process is relatively complicated, the production conditions are harsh, and the yield is low. Contents of the invention [0003] The purpose of the present invention is to overcome the deficiencies of the prior ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08
Inventor 毛晓宇
Owner ANQING FENGYUAN CHEM
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