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Preparation technology of 2-methyl-5-trimethylsiloxyfuran

A technology of trimethylsiloxyfuran and methyl group, which is applied in the field of preparation technology of 2-methyl-5-trimethylsiloxyfuran, can solve problems such as yield limitation, reduce production cost and improve Economic benefits and high productivity

Active 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

[0003] , the usual conjugated diene undergoes 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

[0023] (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;

[0024] (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;

[0025] (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;

[0026] (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;

[0027] (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

[0029] (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;

[0030] (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;

[0031] (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;

[0032] (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;

[0033] (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

[0035] (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;

[0036] (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;

[0037] (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;

[0038] (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;

[0039] (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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Abstract

The invention relates to the field of production of chemical engineering reagents, and especially relates to a preparation technology of 2-methyl-5-trimethylsiloxyfuran. The preparation chemical equation of 2-methyl-5-trimethylsiloxyfuran 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-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 appli...

Claims

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Application Information

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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
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