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Preparation process of 2-methyl-5-trimethylsiloxyfuran

A technology of trimethylsiloxyfuran and a preparation process, which is applied in the field of preparation technology of 2-methyl-5-trimethylsiloxyfuran, can solve problems such as yield limitation, and achieves reduction of production cost and yield. The effect of high rate, green production process and environmental protection

Active Publication Date: 2018-02-13
XINYAQIANG SILICON CHEM JIANGSU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] , the usual conjugated dienes undergo Diels-Alder reaction, the reaction conditions are relatively strict and the reaction is reversible, so the yield is limited

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Under the protection of dry nitrogen and at room temperature, add 0.3g of anhydrous zinc chloride and 12.3g of dry triethylamine to a 250ml three-necked bottle in turn, and stir vigorously until it becomes a suspension;

[0025] (2) Then add dropwise a pre-configured solution of 9.8g 5-methyl-2(3H)-furanone dissolved in 60ml anhydrous tetrahydrofuran into the reaction bottle, and stir for 1 hour after the drop;

[0026] (3) Continue to add 15.5ml of trimethylchlorosilane dropwise to the reaction bottle, after the drop is completed, stir at room temperature for 4 hours to obtain the mixture;

[0027] (4) Then pour the mixture prepared in step (3) into a 1L flask filled with 200ml of n-heptane in advance, stir well, let stand, precipitate, and filter out the insoluble matter Et 3 N HCl;

[0028] (5) Finally, the filtrate was concentrated under reduced pressure at a pressure of 80-100 mmHg, and excess trimethylchlorosilane, tetrahydrofuran, triethylamine and n-heptane...

Embodiment 2

[0030] (1) Under the protection of dry nitrogen and at room temperature, add 10g of anhydrous zinc chloride and 495g of dry triethylamine to a 3000ml three-necked bottle in turn, and stir vigorously until it becomes a suspension;

[0031] (2) Then add dropwise a pre-configured solution of 400g 5-methyl-2(3H)-furanone dissolved in 2040ml anhydrous tetrahydrofuran into the reaction bottle, and stir for 1.5 hours to react;

[0032] (3) Continue to add 620.7ml of trimethylchlorosilane dropwise to the reaction bottle, after the drop is completed, stir at room temperature for 6 hours to obtain the mixture;

[0033] (4) Then pour the mixture prepared in step (3) into a flask filled with 6528ml of n-heptane in advance, stir well, let stand, precipitate, and filter out the insoluble matter Et 3 N HCl;

[0034] (5) Finally, the filtrate was concentrated under reduced pressure at a pressure of 80-100mmHg, and excess trimethylchlorosilane, tetrahydrofuran, triethylamine and n-heptane wer...

Embodiment 3

[0036] (1) Under the protection of dry nitrogen and at room temperature, add 20g of anhydrous zinc chloride and 1000g of dry triethylamine to a 10L three-necked flask in sequence, and stir vigorously until it becomes a suspension;

[0037] (2) Then add dropwise a pre-configured solution of 800g 5-methyl-2(3H)-furanone dissolved in 3.5L anhydrous tetrahydrofuran into the reactor, and stir for 2 hours to react;

[0038] (3) Continue to add 1.3 L of trimethylchlorosilane dropwise to the reaction kettle, after the drop is completed, stir at room temperature for 8 hours to obtain a mixture;

[0039] (4) Then pour the mixture prepared in step (3) into a flask filled with 12L n-heptane in advance, stir well, let stand, precipitate, and filter out the insoluble matter Et 3 N HCl;

[0040] (5) Finally, the filtrate was concentrated under reduced pressure at a pressure of 80-100 mmHg, and excess trimethylchlorosilane, tetrahydrofuran, triethylamine and n-heptane were distilled in seque...

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PUM

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Abstract

The present invention relates to the field of production and preparation of chemical reagents, in particular to the preparation process of 2-methyl-5-trimethylsilyloxyfuran. The chemical formula for the preparation of 2-methyl-5-trimethylsilyloxyfuran is: The molecular formula of the product obtained is: . The compound solvent of tetrahydrofuran and n-heptane is used in the preparation process of the invention, no toxic and harmful substances are produced, the production process is green and environmentally friendly, the yield is high, the production cost of the enterprise is reduced, and the economic benefit of the enterprise is greatly improved.

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-methyl-5-trimethylsilyloxyfuran. Background technique [0002] Diels-Alder reaction (Diels-Alder), the reaction of conjugated diene and olefin to form a six-membered ring is an important organic synthesis reaction, and it is also one of the commonly used reactions in modern drug synthesis. Through this reaction, Cyclic compound molecules that are difficult to prepare by other methods can be prepared, and the reaction formula is: [0003] , the usual conjugated dienes undergo Diels-Alder reaction, the reaction conditions are relatively strict and the reaction is reversible, so the yield is limited. [0004] When the Diels-Alder reaction is carried out through the conjugated diene substituted by alkylsiloxy group, the reaction is usually easy to carry out, and the reaction is irreversible, which greatly improves the applic...

Claims

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Application Information

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Patent Type & Authority Patents(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