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A kind of method for preparing 2-acetylfuran from ketene

A technology of acetylfuran and ketene, applied in the production field of chemical intermediate 2-acetylfuran, can solve the problems of low reactor production efficiency, low raw material utilization rate and high production cost, and achieves low corrosion, low raw material cost, three wastes The effect of low emissions

Active Publication Date: 2015-10-21
SHANDONG HUIHAI PHARMA & CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the raw material utilization rate of this method is too low (the utilization rate of acetic anhydride is only 50%), the production efficiency of the reactor is low, and the production cost is too high

Method used

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  • A kind of method for preparing 2-acetylfuran from ketene

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 136g of furan, 1.0g of phosphoric acid, and 260g of chloroform into a four-necked flask equipped with an electric stirrer, a ketene gas pipe, a thermometer and an exhaust pipe, start stirring, and feed 85g of ketene within 3 hours at 15°C . After the solvent was recovered under normal pressure, rectification was carried out under reduced pressure. At -0.099Mpa, the 78-81°C fraction was collected to obtain 210.2g of 2-acetylfuran with a purity of 99% (the yield was 95.5% based on furan).

[0024] After solvent recovery is directly applied mechanically 6 times, the impact of recovery solvent mechanical application on product yield and purity is shown in the following table:

[0025] Apply times Yield(%) purity(%) 1 95.0 99.3 2 95.3 99.1 3 95.2 99.2 4 95.0 99.4 5 95.2 99.2 6 95.1 99.1

Embodiment 2

[0027] Add 68g of furan, 0.5g of phosphoric acid, and 150g of dichloromethane into a four-necked flask equipped with an electric stirrer, a ketene gas tube, a thermometer, and an exhaust pipe, start stirring, and feed ethylene at 20°C within 3 hours. Ketones 42.0g. After the solvent was recovered under normal pressure, rectification was carried out under reduced pressure. At -0.099Mpa, the 78-81°C fraction was collected to obtain 104.8g of 2-acetylfuran with a purity of 99.1% (the yield was 95.2% based on furan). .

Embodiment 3

[0029] Add 136g of furan, 1.0g of phosphoric acid, and 280g of dichloromethane into a four-necked flask equipped with an electric stirrer, a ketene gas tube, a thermometer, and an exhaust pipe, start stirring, and feed ethylene at 20°C within 3 hours. Ketones 86g. After the solvent was recovered under normal pressure, rectification was carried out under reduced pressure. At -0.099Mpa, the 78-81°C fraction was collected to obtain 209g of 2-acetylfuran with a purity of 99.3% (the yield was 95.0% based on furan).

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Abstract

The invention provides a method for preparing 2-furyl-methylketon from ethenone. In the presence of an acylation catalyst, furan and ethenone react in an organic solvent for 2-5 hours at 5-20 DEG C to prepare crude 2-furyl-methylketon, then the organic solvent is recycled through distillation and the 2-furyl-methylketon is prepared through rectification; the acylation catalyst is one or more of phosphoric acid, sulfuric acid and p-toluenesulfonic acid; the mass ratio of the acylation catalyst to furan is (0.005-0.009) to 1; the organic solvent is one or more of methylene dichloride, ethylene dichloride and chloroform. Compared with the prior art, the method has the advantages and benefits as follows: 1. the method is suitable for continuous production owing to lower raw material cost; 2. the method is suitable for industrial production due to lower reaction temperature; 3. no hydrogen chloride or acetic acid is produced in the production process, the corrosion is light and the discharge of three wastes is low; 4. the solvent can be used directly and indiscriminately after being recycled so as to realize green synthesis, the product yield is up to 95.0% and the purity is up to 99%.

Description

technical field [0001] The invention relates to a production method of a chemical intermediate 2-acetylfuran. Background technique [0002] 2-Acetylfuran is an important intermediate of medicine, pesticide and spice, and the main raw material for the synthesis of furan ammonium salt. [0003] The synthesis process of 2-acetylfuran mainly includes acetic acid method: Helvetica Chimica Acta, 88(8), 2232-2287, 2005, Tetrahedron, 60(48), 10843-10850, 2004, Synthesis, (13), 2165-2168, Mentioned in 2004; Acetyl chloride method: Mentioned in Synthetic Communications, 38(2), 255-264, 2008; Acetic anhydride method: Mentioned in Chinese Journal of Antibiotics 30(5), 304-313, 2005, CN101357910A, etc. . [0004] The acetic acid method has low product conversion rate and yield, up to 40% based on furan, severe corrosion, high production cost and low product quality. [0005] The acetyl chloride route uses acetyl chloride as an acylating agent, and reacts at a lower temperature to gene...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/46
CPCC07D307/46
Inventor 卢言建郑庚修夏青孙成斌张世凤
Owner SHANDONG HUIHAI PHARMA & CHEM
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