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Preparation method of cyclopentanone-2-carboxylic acid methyl ester

A technology for methyl carboxylate and cyclopentanone, which is applied in the field of preparation of cyclopentanone-2-methyl carboxylate, can solve the problems of complex production, high production cost, low yield and the like, and achieves low production cost and high yield , the process produces simple effects

Active Publication Date: 2013-10-02
怀化泰通新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But because the process production of prior art is complicated, and production cost is high, so output is low, can't satisfy the demand of market

Method used

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  • Preparation method of cyclopentanone-2-carboxylic acid methyl ester

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Experimental program
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Effect test

Embodiment 1

[0012] The preparation method of cyclopentanone-2-carboxylate methyl ester, comprises the following steps:

[0013] (1) First, pump DMF into the DMF high-level tank, start stirring, add 1000kg of DMF and 120kg of sodium methoxide into the reaction kettle, continue stirring for 20 minutes after feeding, make it fully stirred, and then raise the temperature in the kettle to 90°C Then add 300kg of diethyl adipate dropwise, keep the temperature under reflux for 8 hours after the dropwise addition, and condense and recover by-product methanol at the same time;

[0014] (2) After the reaction, the solvent DMF was evaporated under reduced pressure. After the solvent was evaporated, the temperature of the reactor was lowered to 40°C, and then 800 kg of toluene was added to stir vigorously for a period of time. After the materials were fully dispersed, 200 kg of 30% hydrochloric acid and water were added. 80kg for acidification reaction; after the acidification reaction, the static lay...

Embodiment 2

[0017] The preparation method of cyclopentanone-2-carboxylate methyl ester, comprises the following steps:

[0018] (1) First, pump DMF into the DMF high-level tank, start stirring, add 1050kg of DMF and 130kg of sodium methoxide into the reaction kettle, continue stirring for 30 minutes after feeding, make it fully stirred, and then raise the temperature in the kettle to 100°C Then, add 400kg of diethyl adipate dropwise, keep the temperature under reflux for 9 hours after the dropwise addition, and condense and recover by-product methanol at the same time;

[0019] (2) After the reaction, the solvent DMF was evaporated under reduced pressure. After the solvent was evaporated, the temperature of the reactor was lowered to 50°C, and then 1000 kg of toluene was added and stirred vigorously for a period of time. After the materials were fully dispersed, 300 kg of 30% hydrochloric acid and water were added. 100kg for acidification reaction; after the acidification reaction, the st...

Embodiment 3

[0021] The preparation method of cyclopentanone-2-carboxylate methyl ester, comprises the following steps:

[0022] (1) First, pump DMF into the DMF high-level tank, start stirring, add 1100kg of DMF and 140kg of sodium methoxide into the reaction kettle, continue stirring for 40 minutes after feeding, make it fully stirred, and then raise the temperature in the kettle to 110°C Then, add 500 kg of diethyl adipate dropwise, keep the temperature under reflux for 10 hours after the dropwise addition, and condense and recover by-product methanol at the same time;

[0023] (2) After the reaction, the solvent DMF was evaporated under reduced pressure. After the solvent was evaporated, the temperature of the reactor was lowered to 60°C, and then 1200kg of toluene was added to stir vigorously for a period of time. After the materials were fully dispersed, 400kg of 30% hydrochloric acid and water were added. 120kg for acidification reaction; after the acidification reaction, the static...

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Abstract

The invention relates to the technical field of cyclopentanone-2-carboxylic acid methyl ester, in particular to a preparation method of cyclopentanone-2-carboxylic acid methyl ester. The method includes: firstly pumping DMF into a DMF elevated tank, starting stirring, adding 1000-1100kg of DMF and 120-140kg of sodium methoxide into a reaction kettle, then further conducting stirring for 20-40min to make the materials fully mixed uniformly, then raising the temperature in the kettle to about 90-110DEG C, then adding 300-500kg of diethyl adipate dropwisely, then keeping the temperature and performing a reflux reaction for 8-10h. The method provided in the invention adopts DMF as a main plate material, and at the same time adds various auxiliary materials to prepare the product. The finished product yield is up to 99%, the output is high, and the exhaust gas and the distillation residue generated in the production process are both effectively treated, thus avoiding environmental pollution. Also, the finished product can be widely used in industries of daily cosmetics, medicines, pesticides and food. In addition, the method involved in the invention has the characteristics of simple production process, low production cost, and high yield, etc.

Description

technical field [0001] The invention relates to the technical field of methyl cyclopentanone-2-carboxylate, in particular to a preparation method of methyl cyclopentanone-2-carboxylate. Background technique [0002] Methyl cyclopentanone-2-carboxylate has a fruity aroma and can be used as a fragrance in the daily cosmetics industry. In the pharmaceutical industry, it can be used to synthesize cardiovascular preparations, prostaglandins and cephalosporin antibiotics, mitomycin, etc. It is also an intermediate of loxoprofen sodium, and can be used to synthesize phenyluracil herbicides in the pesticide industry. The food industry can synthesize milk-flavored flavors, and a series of milk-flavored flavors can be synthesized through methyl cyclopentanone-2-carboxylate. Because this flavor has a natural milky flavor, the fragrance is soft and long-lasting, it has been widely used at present. Applied in various food flavors, the market prospect is very broad. But because the proc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/757C07C67/313
Inventor 储晓建
Owner 怀化泰通新材料科技有限公司