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Method for synthesizing 2-acetylfuran

A technology for acetylfuran and furan, applied in the field of compound synthesis, can solve the problems of difficult recovery of acetic anhydride, difficult separation, increased cost and the like, and achieves the effects of saving reagent consumption, improving operating environment and saving costs

Inactive Publication Date: 2009-02-04
JIANGSU QINGQUAN CHEM CO LTD
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0004] Among the above-mentioned documents, the method for synthesizing 2-acetylfuran has: Chinese Journal of Antibiotics 30 (5), 304,313, and the mol ratio of acetic anhydride and furan in the technology introduced in 2005 is 1.57: 1, then react under catalyst catalysis, The yield is up to 95%, but the process uses a large amount of excess acetic anhydride, which is difficult to recover, resulting in separation difficulties and increased costs
[0005] Indian, 192962, 19 Jun 2004 mentioned Fe 3+ The exchanged montmorillonite is used as a catalyst, furan is used as a solvent for acylation reaction, and the yield reaches 98%.
[0006] Chemical Reagents, 23(6), 370-371, 2001 introduction with dichloroethane as solvent, phosphoric acid as catalyst, equimolar furan and acetic anhydride reaction yield is 40%, its reaction process will use a large amount of dichloroethane The reagent is used as a solvent, and the yield is low and the cost is high

Method used

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  • Method for synthesizing 2-acetylfuran
  • Method for synthesizing 2-acetylfuran
  • Method for synthesizing 2-acetylfuran

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Add 12.3g (0.12mol) of acetic anhydride and 1.2g of 85% phosphoric acid into a 100mL flask equipped with electric stirring, a thermometer, and a condenser, and add 6.8g (0.1mol) of furan dropwise at 25°C for about 1 hour while stirring, Then the temperature was raised to 70°C for 5h. Then cool to 50°C and add 200mL of water, stir for 0.5h, cool to below 30°C and extract three times with 100mL of chloroform, and combine the extracts. The extract was neutralized with 30% liquid caustic soda to about pH 6.5, the organic layer was separated, and the organic layer was washed with water until neutral. The organic layer was distilled under normal pressure to recover chloroform, and then vacuum distillation collected the cuts at 65-70°C / 12mmHg to obtain 9.8g of product with a yield of 89.0%. The purity of 2-acetylfuran reached 99.2% by gas phase analysis. 2, 5-Diacetylfuran 0.1%, acetic acid 0.7%.

[0034] The mass spectrum of 2-acetylfuran (using Agilent Technologies 5973 Ne...

Embodiment 2

[0036] The dosage of acetic anhydride was changed to 13.3g (0.13mol), and the others were the same as in Example 1. The result was 9.9g of 2-acetylfuran, a yield of 90.0%, and a gas-phase purity of 99.0%. The mass spectrum of the product is shown in Example 1.

Embodiment 3

[0038] The dosage of acetic anhydride was changed to 11.2g (0.11mol), and the others were the same as in Example 1. The result was 9.7g of 2-acetylfuran, the yield was 88.2%, and the gas phase purity was 99.2%. The mass spectrum of the product is shown in Example 1.

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Abstract

The invention relates to a method for synthesizing 2-acetyl furan, comprising the following steps: catalyst and acetic anhydride are mixed and stirred evenly; furan is added into the mixture in drops; temperature reaction is carried out; then the reaction solution is cooled, added with water and is extracted by a solvent for three times, and the extracting layers are combined; the combined solution is washed in alkali and water sequentially, and the solvent is distilled under normal pressure or reduced pressure, and the product is collected by reduced pressure distillation. The method has the advantages of mild reaction condition, saving the amount of materials, simple and purified products and high yield.

Description

technical field [0001] The invention relates to the technical field of compound synthesis methods, in particular to a method for synthesizing 2-acetylfuran. Background technique [0002] Acetyl furan and its derivatives can be used as food additives, as well as initial raw materials and intermediates of medicine, pesticides and spices. At present, there are mainly the following methods for the synthesis of acetylfuran: [0003] The common method for synthesizing 2-acetylfuran is to carry out the method for acetylation with furan, and the acylating agent of prior art has the acetyl chloride mentioned in Synthetic Communications, 38 (2), 255-264,2008; Chinese Journal of Antibiotics 30 (5), 304, 313, 2005, Indian, 192962, 19 Jun 2004, etc. mentioned acetic anhydride; Helvetica Chimica Acta, 88(8), 2282-2287, 2005, Tetrahedron, 60(48), 10843-10850, acetic acid mentioned in 2004, Synthesis, (13), 2165-2168, 2004, etc. [0004] Among the above-mentioned documents, the method fo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/46
Inventor 刘建华杨荣强聂振中陈欣荣潘志伟任松高广居
Owner JIANGSU QINGQUAN CHEM CO LTD