Method for preparing 2-furyl-methylketon from ethenone
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A technology of acetylfuran and ketene, applied in the production field of chemical intermediate 2-acetylfuran, which can solve the problems of low reactor production efficiency, low raw material utilization rate, and high production cost, and achieve low corrosion, low raw material cost, and three wastes The effect of reducing emissions
Active Publication Date: 2014-03-26
SHANDONG HUIHAI PHARMA & CHEM
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However, the raw material utilization rate of this method is too low (the utilization rate of acetic anh
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Embodiment 1
[0023] Add 136g furan, 1.0g phosphoric acid and 260g chloroform into a four-necked flask equipped with electric stirring, ketene gas tube, thermometer and vent tube, turn on the stirring, and pour 85g ketene within 3 hours at 15℃ . After recovering the solvent under normal pressure, rectifying under reduced pressure, collecting 78-81°C fractions at -0.099Mpa to obtain 210.2g of 2-acetylfuran with a purity of 99% (the yield is 95.5% based on furan).
[0024] After the solvent recovery is directly applied for 6 times, the effect of recovered solvent applied on the product yield and purity is shown in the following table:
[0025] Number of applications Yield(%) purity(%) 195.099.3 295.399.1 395.299.2 495.099.4 595.299.2 695.199.1
Embodiment 2
[0027] In a four-necked flask equipped with electric stirring, ketene gas tube, thermometer and exhaust tube, add 68g furan, 0.5g phosphoric acid, 150g dichloromethane, turn on the stirring, and pour ethylene within 3 hours at 20℃ Ketone 42.0g. After recovering the solvent at normal pressure, rectifying under reduced pressure, collecting 78-81°C fractions at -0.099Mpa to obtain 104.8 g of 2-acetylfuran with a purity of 99.1% (the yield is 95.2% based on furan). .
Embodiment 3
[0029] In a four-necked flask equipped with electric stirring, ketene gas tube, thermometer and exhaust tube, add 136g furan, 1.0g phosphoric acid, 280g methylene chloride, turn on the stirring, and pour ethylene within 3 hours at 20℃ Ketone 86g. After recovering the solvent under normal pressure, rectifying under reduced pressure, collecting 78-81°C fractions at -0.099Mpa to obtain 209 g of 2-acetylfuran with a purity of 99.3% (the yield is 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 chemical intermediate 2-acetylfuran. Background technique [0002] 2-Acetylfuran is an important intermediate of medicines, pesticides and perfumes, and is the main raw material for the synthesis of furan ammonium salt. [0003] The synthesis process of 2-acetylfuran mainly includes the acetic acid method: Helvetica Chimica Acta, 88(8), 2232-2287, 2005, Tetrahedron, 60(48), 10843-10850, 2004, Synthesis, (13), 2165-2168, Mentioned in 2004, etc.; 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 conversion rate and yield of acetic acid process products are low, up to 40% based on furan, with serious corrosion, high production cost and low product quality. [0005] The acetyl chloride route uses acetyl chloride as the acylating agent, and reacts at a lower te...
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