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Preparation method of 2-acetylfuran

A technology for acetylfuran and furanmethyl alcohol, which is applied in the field of preparation of 2-acetylfuran, can solve the problems of restricting product market stability, poor atomic economic efficiency, and high safety risks, and achieves low production cost, satisfactory stability, and high catalyst performance. simple effect

Active Publication Date: 2021-06-22
长沙启晟合研医药科技有限公司
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Problems solved by technology

[0003] At present, the synthesis method of 2-acetylfuran in industry basically uses furfural as the starting material. First, furfural is oxidized to furoic acid, then furoic acid is decarboxylated in the presence of a catalyst to become furan, and then furan is produced by reacting with acetic anhydride under acid catalysis. 2-Acetyl furan, this process not only seriously pollutes the three wastes, but also has poor atomic economic benefits, and more importantly, the key intermediate furan in the production process has a boiling point of only over 30 degrees, which is flammable and explosive, and has a very high safety risk, which is seriously restricted. market stability of the product

Method used

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  • Preparation method of 2-acetylfuran
  • Preparation method of 2-acetylfuran
  • Preparation method of 2-acetylfuran

Examples

Experimental program
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Effect test

Embodiment 12

[0034] The preparation method of embodiment 12-acetylfuran

[0035] 1. Format response:

[0036] Add 100 ml of tetrahydrofuran solution of 3 moles per liter of methylmagnesium chloride to the reactor, cool down to about zero, slowly add 25 ml of furfural, keep the internal temperature not exceeding 25 ° C, and slowly drop the reaction solution after the reaction is completed. Add it to 100 ml of ice water, control the internal temperature not to exceed 25°C, then slowly add dilute hydrochloric acid dropwise to adjust the pH of the reaction solution to about 7, separate the organic layer, and then concentrate to dryness to obtain furan methyl alcohol. 99%.

[0037] 2. Oxidation reaction:

[0038] Add 100 milliliters of ethylene dichloride, 27.5 grams of furan methyl alcohol, 0.8 gram of 4-hydroxyl-2,2,6,6-tetramethylpyridine oxide (Temp), 0.6 gram of potassium bromide in the reactor, Control the temperature at 25° C. and feed air or oxygen to react for 3 to 5 hours. After th...

Embodiment 2-5

[0041] The difference from Example 1 is that the solvent used in the oxidation reaction is different: dichloromethane, trichloromethane, tetrahydrofuran or acetonitrile are used instead of dichloroethane.

Embodiment 6-10

[0043] The difference from Example 1 is that the temperature of the oxidation reaction is different: the temperatures are 0, 10°C, 20°C, 30°C, and 40°C, respectively.

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Abstract

The invention discloses a preparation method of 2-acetylfuran, which comprises the following steps: taking furfural as a raw material, carrying out Grignard reaction to obtain furfuryl alcohol, and carrying out oxidation reaction on furfuryl alcohol in the presence of a catalyst in an oxygen-containing atmosphere to obtain 2-acetylfuran, wherein the catalyst is a 4-hydroxy-2, 2, 6, 6-tetramethylpyridine oxide (Temp) and potassium bromide. The method is simple in process, simple in catalyst and suitable for large-scale industrial production, the stability meets the market requirements of products, the product cost is lower than that of existing industrial production, and the product quality is better.

Description

technical field [0001] The invention belongs to the field of compound synthesis, and in particular relates to a preparation method of 2-acetylfuran. Background technique [0002] 2-Acetyl furan is an important organic synthetic material and is widely used in industrial production. 2-Acetylfuran can be used in the synthesis of cefuroxime axetil, cefuroxime, furonicazone and other drugs in medicine, and it is mainly used as an additive in soup, meat, condiments, etc. in the food industry. [0003] At present, the synthesis method of 2-acetylfuran in industry basically uses furfural as the starting material. First, furfural is oxidized to furoic acid, then furoic acid is decarboxylated in the presence of a catalyst to become furan, and then furan is produced by reacting with acetic anhydride under acid catalysis. 2-Acetyl furan, this process not only seriously pollutes the three wastes, but also has poor atomic economic benefits, and more importantly, the key intermediate fura...

Claims

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Application Information

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IPC IPC(8): C07D307/46B01J31/26
CPCC07D307/46B01J27/08B01J31/0244B01J31/0271B01J31/26B01J2231/70
Inventor 郑良彬
Owner 长沙启晟合研医药科技有限公司
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