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A kind of cyclopropionyl acetone and its synthetic method

A technology of cyclopropionyl acetone and its synthesis method, which is applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of carbonyl compounds by condensation, etc., and can solve the problems of low reaction yield, high recovery energy consumption, and large energy consumption. , to achieve the effects of saving raw material costs, low environmental requirements, and high catalytic efficiency

Active Publication Date: 2021-12-28
陕西恒润化学工业有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The condensation reaction between molecules of different substances is carried out in alkali, and there are many by-products of the reaction, so the yield of the reaction is not high, only about 75%, resulting in high production costs for the enterprise
[0003] In the synthesis process of cyclopropionyl acetone, sodium hydride is used as a catalyst, but the requirements for sodium hydride are high. The entire environmental reaction process, including solvents and raw materials, must be absolutely anhydrous, otherwise sodium hydride reacts with water to generate extremely dangerous gas hydrogen. Flammable, explosive, and powerful, and toluene is used as a solvent in the synthesis process. Toluene is highly toxic, unsafe, and requires a lot of energy for recycling
Therefore, in the existing cyclopropionyl acetone synthesis process, the safety is poor, the equipment environment requirements are high, the energy consumption is large, the yield is low, and the cost is high, which is not conducive to large-scale production of enterprises

Method used

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  • A kind of cyclopropionyl acetone and its synthetic method

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Embodiment 1

[0031] A synthetic method for cyclopropionyl acetone, comprising the following steps:

[0032] Step 1, add 500kg of 98% absolute ethanol in the reactor, stir with the rotating speed of 95 rpm at room temperature, add 46kg sodium metal in batches while stirring (add sodium metal once every 10 minutes, divide 9 times Adding), in the process of adding sodium metal, the temperature was controlled at 64°C by opening the jacket to cool down the water, and then the temperature was raised to 78°C for 1 hour to completely dissolve the sodium metal, and the ethanol was recovered under normal pressure at 78°C for 2 hours. After recovering 350kg of ethanol, a mixed solution of sodium ethylate and ethanol was obtained.

[0033] Step 2, add 170kg of cyclopropyl methyl ketone to the mixed solution, stir at 60°C at a speed of 95 rpm for 30 minutes, add 88kg of ethyl acetate, and reflux at 60°C for 1 hour. Slowly heat up to 78°C within 30 minutes and recover 150kg of ethanol under normal pres...

Embodiment 2

[0038] A synthetic method for cyclopropionyl acetone, comprising the following steps:

[0039] Step 1, add 480kg of 98% absolute ethanol in the reactor, stir with the rotating speed of 95 revs / min at room temperature, add 46kg metallic sodium in batches while stirring (add 4.5kg of metallic sodium once every 10 minutes, divide 9 additions), during the process of adding sodium metal, the temperature was controlled at 65°C by opening the jacket to cool down the water, and then the temperature was raised to 80°C for 1.2 hours to completely dissolve the sodium metal, and 1.7 ethanol was recovered under normal pressure at 79°C Hour, after ethanol reclaims 350kg, get the mixed liquor of sodium ethylate and ethanol.

[0040] Step 2, add 180kg of cyclopropyl methyl ketone to the mixed solution, stir at a speed of 95 rpm at 55°C for 25 minutes, add 86kg of ethyl acetate, and reflux at 55°C for 1.2 hours. Slowly heat up to 79°C within 30 minutes and recover 150kg of ethanol under norma...

Embodiment 3

[0044] A synthetic method for cyclopropionyl acetone, comprising the following steps:

[0045] Step 1, add 520kg of 98% absolute ethanol in the reactor, stir with the rotating speed of 95 revs / min at room temperature, add 46kg metallic sodium in batches while stirring (add 5.5kg of metallic sodium once every 10 minutes, divide 9 additions), during the process of adding sodium metal, the temperature was controlled at 62°C by opening the jacket to cool down the water, and then the temperature was raised to 79°C for 1.5 hours to completely dissolve the sodium metal, and 1.5 ethanol was recovered under normal pressure at 80°C. Hour, after ethanol reclaims 350kg, get the mixed liquor of sodium ethylate and ethanol.

[0046] Step 2, add 160kg of cyclopropyl methyl ketone to the mixed solution, stir at 60°C at a speed of 95 rpm for 30 minutes, add 90kg of ethyl acetate, and reflux at 50°C for 1.5 hours. Slowly heat up to 80°C within 35 minutes and recover 150kg of ethanol under norm...

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Abstract

The invention discloses a cyclopropionyl acetone and a synthesis method thereof, which comprises the following steps: adding sodium to absolute ethanol while stirring, lowering the temperature, reacting, and recovering ethanol to obtain a mixed solution; adding cyclopropylmethyl to the mixed solution Base ketone, stir, add 1 / 3 mass of ethyl acetate, reflux reaction, reclaim ethanol; then lower the temperature, add 1 / 3 mass of ethyl acetate, reflux reaction, reclaim ethanol; cool down again, add 1 / 3 mass of acetic acid Ethyl ester, reflux reaction, recovery of ethanol and ethyl acetate under negative pressure, cooling and storage, to obtain cyclopropyl methyl ketone sodium salt solution; adjust the pH of cyclopropyl methyl ketone sodium salt solution to 2~3, stir, and let stand , Take the upper layer of brownish-red liquid, and fractionally distill it to obtain cyclopropionyl acetone. The content of the obtained cyclopropionylacetone is about 90%, and the yield is greater than 90%. The synthesis method has mild reaction conditions, high catalytic efficiency, low energy consumption, low cost, easy recovery of the product, good safety, and is suitable for large-scale production of enterprises. .

Description

technical field [0001] The invention relates to the technical field of synthesis and application of fine chemical products, in particular to cyclopropionylacetone and a synthesis method thereof. Background technique [0002] In the synthesis process of cyprodinil, there is a one-step reaction called the Claisen reaction. The Claisen condensation reaction refers to the condensation of esters containing α-hydrogen under the action of alkaline condensing agents such as sodium alkoxide, and the loss of a molecule of alcohol The reaction to give β-ketoesters is called Claisen condensation. The condensation reaction between molecules of different substances is carried out in alkali, and there are many reaction by-products, so the yield of the reaction is not high, only about 75%, which leads to higher production costs of the enterprise. [0003] In the synthesis process of cyclopropionyl acetone, sodium hydride is used as a catalyst, but the requirements for sodium hydride are hi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/45C07C49/293
CPCC07C45/455C07C2601/02C07C49/293
Inventor 樊明李仓珍谌敦国晁六民王建桥尹炜新
Owner 陕西恒润化学工业有限公司
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