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Preparation technology of 2,5-bis(trimethylsiloxy)-3-methylfuran

A technology of trimethylsiloxy and methylfuran, which is applied in the field of preparation technology of 2,5-bis(trimethylsiloxy)-3-methylfuran, can solve problems such as yield limitation, and achieves The effect of reducing production cost, high yield and improving economic efficiency

Inactive Publication Date: 2015-10-21
XINYAQIANG SILICON CHEM JIANGSU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The Diels-Alder reaction of the usual conjugated diene is relatively strict, and the reaction is reversible, so the yield is also limited.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Under the protection of dry nitrogen and at room temperature, add 0.5g of anhydrous zinc chloride and 29g of dry triethylamine to a 250ml three-necked flask, and stir vigorously until it becomes a suspension;

[0027] (2) Then drop a pre-prepared solution of 11.4g methyl succinic anhydride dissolved in 80ml anhydrous tetrahydrofuran into the reaction flask, and then stir the reaction for 1 hour;

[0028] (3) Continue to add 31 g of trimethylchlorosilane dropwise to the reaction flask, and after the drop is completed, stir at room temperature for 4 hours to obtain a mixture;

[0029] (4) Pour the mixture obtained in step (3) into a flask containing 300ml n-heptane, stir thoroughly, and then stand still. After the precipitation is sufficient, filter out the insoluble triethylamine hydrochloride (Et 3 N·HCl);

[0030] (5) Concentrate under reduced pressure, and distill out the excess trimethylchlorosilane, tetrahydrofuran,

[0031] With triethylamine and n-heptane, 23.4 g of 2,5...

Embodiment 2

[0033] (1) Under the protection of dry nitrogen and at room temperature, add 11.95g of anhydrous zinc chloride and 496.6g of dry triethylamine to the 0.8L reactor in sequence, and stir vigorously until it becomes a suspension;

[0034] (2) Then, add a pre-configured solution of 200g methyl succinic anhydride dissolved in 5.4L anhydrous tetrahydrofuran into the reaction flask dropwise, after the drop is completed, the reaction is stirred for 1.5 hours;

[0035] (3) Continue to add 533.2 g of trimethylchlorosilane dropwise to the reaction flask, and after the drop is completed, stir at room temperature for 7.5 hours to obtain a mixture;

[0036] (4) Pour the mixture obtained in step (3) into a flask containing 4.73L n-heptane, stir thoroughly, and then stand still. After the precipitation is sufficient, filter out the insoluble triethylamine hydrochloride (Et 3 N·HCl);

[0037] (5) Concentrate under reduced pressure, distill out the excess trimethylchlorosilane, tetrahydrofuran,

[0038] ...

Embodiment 3

[0040] (1) Under the protection of dry nitrogen and at room temperature, add 40g of anhydrous zinc chloride and 1250g of dry triethylamine to the 10L reactor in sequence, and stir vigorously until it becomes a suspension;

[0041] (2) Then, add a pre-configured solution of 500g methyl succinic anhydride dissolved in 2628ml anhydrous tetrahydrofuran into the reaction flask dropwise. After the drop is completed, the reaction is stirred for 2 hours;

[0042] (3) Continue to add 1332g of trimethylchlorosilane dropwise to the reaction flask, and after the drop is completed, stir at room temperature for 8 hours to obtain a mixture;

[0043] (4) Pour the mixture obtained in step (3) into a flask containing 10.95L n-heptane, stir thoroughly, and then stand still. After the precipitation is sufficient, filter out the insoluble triethylamine hydrochloride (Et 3 N·HCl);

[0044] (5) Concentrate under reduced pressure, and distill out the excess trimethylchlorosilane, tetrahydrofuran,

[0045] With...

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PUM

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Abstract

The invention relates to the field of production of chemical engineering reagents, and especially relates to a preparation technology of 2,5-bis(trimethylsiloxy)-3-methylfuran. The preparation chemical equation of 2,5-bis(trimethylsiloxy)-3-methylfuran is shown in the specification, and the molecular formula of the above obtained product is also shown in the specification. A tetrahydrofuran and n-heptane composite solvent is used in the preparation technology, so the preparation technology has the advantages of no generation of poisonous or harmful substances, green and environmentally-friendly production process, high yield, enterprises' production cost reduction, and great improvement of the enterprises' economic benefits.

Description

technical field [0001] The invention relates to the field of production and preparation of chemical reagents, in particular to a preparation process of 2,5-bis(trimethylsilyloxy)-3-methylfuran. Background technique [0002] The Diels-Alder reaction (Diels-Alder reaction), the reaction of conjugated diene and olefin to form a six-membered ring, is an important organic synthesis reaction and one of the most commonly used reactions in modern drug synthesis. Through this reaction, cyclic compound molecules that are difficult to prepare by other methods can be prepared. The reaction formula is: [0003] [0004] The Diels-Alder reaction of the usual conjugated dienes is relatively strict, and the reaction is reversible, so the yield is also limited. [0005] When the Diels-Alder reaction is carried out through the alkylsiloxy-substituted conjugated diene, the reaction is usually easy to proceed, and the reaction is irreversible, which greatly improves the application of this...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 初亚军刘汉兴李志刚初亚贤刘春山马李慧
Owner XINYAQIANG SILICON CHEM JIANGSU