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Synthetic method of methyl isobutyrylacetate

A technology for the synthesis of methyl isobutyrylacetate, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of carboxylic acid salts, can solve the problems of high energy consumption, high waste, and difficult product separation, and achieve energy efficiency The effect of low consumption and low boiling point

Active Publication Date: 2021-05-28
山东艾孚特科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the boiling point of the product methyl isobutyrylacetate is similar to that of the raw material methyl acetoacetate, it is difficult to separate the product, and it must be rectified to obtain methyl isobutyrylacetate with high purity, resulting in high waste, high environmental protection pressure, and energy high consumption

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0017] In the synthetic method of methyl isobutyryl acetate of the present invention, the catalytic reaction is carried out in a two-necked flask with a volume of 500 mL, equipped with a mechanical stirrer. The steps of the catalytic test are as follows: put 100mmol of acetonitrile, 120mmol of sodium methoxide and 8.21g of p-xylene into the flask, raise the reaction temperature to 80°C, turn on the mechanical stirring, and slowly add 120mmol of isobutyryl chloride dropwise for 2 hours. . After reacting for 10 hours, adjust the pH to 1 with 1.5 mol / L hydrochloric acid, add 100 mmol of methanol, and react for 8 hours at 40°C. After the reaction is completed, separate layers, wash the organic layer with water, wash with saturated sodium bicarbonate, and wash with water until pH=6.5- 7.5 and the material liquid is clean and transparent. Concentrate at normal pressure and then under reduced pressure. After the concentration is complete, the product methyl isobutyrylacetate is obta...

Embodiment 2

[0019] In the synthetic method of methyl isobutyryl acetate of the present invention, the catalytic reaction is carried out in a two-necked flask with a volume of 500 mL, equipped with a mechanical stirrer. The steps of the catalytic test are as follows: put 100mmol of acetonitrile, 100mmol of sodium methoxide and 49.27 g of o-xylene into the flask, raise the reaction temperature to 120°C, start the mechanical stirring, and slowly add 100mmol of isobutyryl chloride dropwise for 2 hours. After reacting for 48 hours, adjust the pH to 1 with 1.5 mol / L hydrochloric acid, add 200 mmol of methanol, and react at 120°C for 15 hours. After the reaction is completed, the layers are separated, and the organic layer is washed with water, saturated sodium bicarbonate, and washed with water until pH=6.5- 7.5 and the material liquid is clean and transparent. Concentrate at normal pressure and then under reduced pressure. After the concentration is complete, the product methyl isobutyrylaceta...

Embodiment 3

[0021] In the synthetic method of methyl isobutyryl acetate of the present invention, the catalytic reaction is carried out in a two-necked flask with a volume of 500 mL, equipped with a mechanical stirrer. The steps of the catalytic test are as follows: put 100mmol of acetonitrile, 120mmol of sodium hydride and 12.318g of o-xylene into the flask, raise the reaction temperature to 90°C, turn on the mechanical stirring, and slowly add 120mmol of isobutyryl chloride dropwise for 2 hours . After reacting for 10 hours, adjust the pH to 1 with 1.5 mol / L hydrochloric acid, add 100 mmol of methanol, and react at 60°C for 10 hours. After the reaction is completed, separate layers, wash the organic layer with water, wash with saturated sodium bicarbonate, and wash with water until pH=6.5- 7.5 and the material liquid is clean and transparent. Concentrate under normal pressure and then under reduced pressure. After the concentration is complete, the product methyl isobutyrylacetate is o...

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Abstract

The invention belongs to the technical field of medicine preparation, and particularly relates to a synthetic method of methyl isobutyrylacetate. The method comprises the following steps: reacting acetonitrile and isobutyryl chloride in a reaction solvent in the presence of a base catalyst to prepare methyl isobutyrylacetate, regulating the pH value to 1 by using hydrochloric acid, adding methanol, carrying out hydrolytic esterification reaction, and separating a product from an organic phase through atmospheric distillation and reduced pressure distillation. The raw material acetonitrile used in the synthetic method of methyl isobutyrylacetate is cheaper, has a low boiling point and is easy to separate from the product, the product can be purified only through reduced pressure distillation after the reaction is finished, and the energy consumption is low.

Description

technical field [0001] The invention belongs to the technical field of medicine preparation, and in particular relates to a method for synthesizing methyl isobutyrylacetate. Background technique [0002] With the rapid development of the global economy and changes in human lifestyles, under the influence of hypertension, hyperlipidemia, and hyperglycemia, the development of cardiovascular diseases such as atherosclerosis has become increasingly prominent in the population. In the treatment of cardiovascular and cerebrovascular diseases, atorvastatin is currently the most effective statin blood lipid regulating drug, which has the greatest effect of lowering low-density lipoprotein (LDL-C) and the strongest effect of lowering triglycerides, and can Raising high-density lipoprotein cholesterol (HDI-C) levels is the only statin drug proven to reduce cardiovascular events better than revascularization. Methyl isobutyrylacetate is a key intermediate in the synthesis of atorvasta...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/716
CPCC07C67/08C07C51/08C07C51/353C07C69/716C07C53/08C07C59/185
Inventor 周倜张晓谦相浩龙张立东李继宾何海林张新一宋浩田达魏凤鲁琳琳邢文国周兴波夏明莹周红财董翠翠王海波张丹丹唐凯盛亮亮
Owner 山东艾孚特科技有限公司
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