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Synthesis method of cyclopropyl methyl ketone

A technology of cyclopropyl methyl ketone and synthesis method, which is applied in the preparation of heterocyclic compounds, the preparation of carbon-based compounds, chemical instruments and methods, etc., can solve the problems of complex process, industrial scale, and high production difficulty, and achieve atomic economy. High performance, low cost of raw materials, mild reaction conditions

Active Publication Date: 2020-03-06
SHANGHAI SHENGNONG PESTICIDE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention proposes a cyclopropyl methyl ketone synthesis process complex process, high raw material cost, high difficulty in industrial scale production and other problems in the existing cyclopropyl methyl ketone synthesis process. The synthetic method of methyl methyl ketone

Method used

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  • Synthesis method of cyclopropyl methyl ketone

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Effect test

Embodiment 1

[0032] Synthesis of cyclopropylmethyl ketone: In a 1000ml hydrogenation kettle, add 400g of 2-methylfuran and 100g of water, 2g of 5% palladium carbon catalyst, replace with nitrogen, then replace with hydrogen, stir to control the reaction temperature for 28 ℃, use a hydrogen balloon to continue the hydrogenation reaction, the reaction ends after 3 hours, the reaction solution is filtered after nitrogen replacement, the catalyst can be applied to the next batch, the reaction solution is allowed to stand for stratification, and the water layer can be applied to the next batch; the organic phase is acetyl-n-propane Alcohol 448g, purity 95.3%.

[0033] In a 1000ml three-neck flask, add 340g of 20% hydrochloric acid, heat to 90°C, add dropwise 100g of the above-mentioned acetyl n-propanol, and distill to collect the azeotrope 5-chloro-2-pentanone and dilute acid water. After the dropwise addition, continue to distill until no organic phase is evaporated. After standing and strati...

Embodiment 2

[0036] Synthesis of cyclopropylmethyl ketone: In a 1000ml hydrogenation kettle, add 400g of 2-methylfuran and 100g of water, 2g of 10% palladium carbon catalyst, replace with nitrogen, then replace with hydrogen, stir to control the reaction temperature 30 ℃, continue the hydrogenation reaction with a hydrogen balloon, the reaction ends after 2.5 hours, the reaction solution is filtered after nitrogen replacement, the catalyst can be applied to the next batch, the reaction solution is allowed to stand for stratification, and the water layer can be applied to the next batch; Alcohol 448g, purity 95.5%.

[0037] In a 1000ml three-neck flask, add 340g of 15% hydrochloric acid, heat to 92°C, add dropwise 100g of the above-mentioned acetyl n-propanol, and distill to collect the azeotrope 5-chloro-2-pentanone and dilute acid water. After the dropwise addition, continue to distill until no organic phase evaporates. After standing and layering, the organic phase obtains 130 g of 5-chl...

Embodiment 3

[0040] Synthesis of cyclopropyl methyl ketone: In a 1000ml hydrogenation kettle, add 400g of 2-methylfuran and 100g of water, 2g of 10% palladium carbon catalyst, replace with nitrogen, then replace with hydrogen, stir to control the reaction temperature 25 ℃, continue the hydrogenation reaction with a hydrogen balloon, the reaction ends after 2 hours, the reaction solution is filtered after nitrogen replacement, the catalyst can be applied to the next batch, the reaction solution is allowed to stand for stratification, and the water layer can be applied to the next batch; Alcohol 448g, purity 95.2%.

[0041] In a 1000ml three-neck flask, add 340g of 20% hydrochloric acid, heat to 95°C, add dropwise 100g of the above-mentioned acetyl n-propanol, and distill to collect the azeotrope 5-chloro-2-pentanone and dilute acid water. After the dropwise addition, continue to distill until no organic phase evaporates. After standing and stratifying, the organic phase is 130 g of 5-chloro...

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Abstract

The invention relates to a synthesis method of cyclopropyl methyl ketone. The synthesis method includes the steps of: 1) carrying out hydrogenation hydrolysis on 2-methyl furan in the presence of a hydrogenation catalyst, hydrogen and water by one-pot process to prepare acetyl n-propanol; 2) carrying out hydrochloric acid chlorination reaction on the acetyl n-propanol prepared in step 1) to prepare 5-chloro-2-pentanone; and 3) carrying out ring closing reaction on the crude product of 5-chloro-2-pentanone prepared in step 2) under an alkaline condition to obtain the cyclopropyl methyl ketone.The synthesis method of cyclopropyl methyl ketone provided by the invention adopts 2-methyl furan as the raw material, carries out one-pot process hydrogenation hydrolysis, hydrochloric acid chlorination reaction and ring closing reaction to obtain cyclopropyl methyl ketone, the process is simple and smooth, and the reaction conditions are mild, therefore the synthesis method is suitable for industrial scale-up production; by adopting 2-methylfuran as the raw material, the method is high in atom economy, green and environment-friendly, and low in raw material cost.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a synthesis method of cyclopropyl methyl ketone. Background technique [0002] Cyclopropyl methyl ketone is an important raw material of the fungicide cyproconazole. In the existing synthesis process, there are many problems such as complex process, high cost of raw materials, and high difficulty in industrial scale-up production. As reported in patent CN200610098154 and CN201210099170, 5-chloro-2-pentanone or acetylbutyrolactone is used as raw material, the cost of raw material is too high, and the economic benefit is low; the hydrogenation of 2-methylfuran reported in patent CN201611008606 obtains 2-methylfuran Dihydrofuran is re-isomerized into cyclopropyl methyl ketone, the catalyst is expensive, and the yield is too low, resulting in high raw material costs; and as reported in patent CN201511010127, acetylbutyrolactone is used as raw material, and cyclopropyl is obtained by...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/65C07C49/293
CPCC07C45/59C07C45/63C07C45/65C07C2601/02C07C49/17C07C49/16C07C49/293
Inventor 王涛韩海平方燕耿玉佳董建生毕强张芝平
Owner SHANGHAI SHENGNONG PESTICIDE
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