Preparation method of ethyl benzoylacetate

A technology of ethyl benzoyl acetate and concentrated sulfuric acid, which is applied in the preparation of carboxylic acid esters, the preparation of organic compounds, the separation/purification of carboxylic acid esters, etc., can solve the problems of surface corrosion and affecting filtration efficiency, and achieve enhanced durability Corrosiveness, the effect of guaranteeing the service life

Active Publication Date: 2021-08-03
江苏巨莱生物医药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing preparation method of ethyl benzoyl acetate needs to be filtered after the reaction is completed. After several times of use, the surface of the traditional microporous membrane will be corroded obviously, which will affect the filtration efficiency and product quality.

Method used

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  • Preparation method of ethyl benzoylacetate
  • Preparation method of ethyl benzoylacetate
  • Preparation method of ethyl benzoylacetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The preparation method of ethyl benzoyl acetate comprises the steps:

[0030] Step S1: Add carbon tetrachloride and sodium bicarbonate into the reaction kettle, stir at a speed of 150r / min, and a temperature of 15°C, and add ethyl acetoacetate, after stirring for 10 minutes, add benzoyl chloride, The temperature was raised to 50°C, and the reaction was continued for 3 hours;

[0031] Step S2: Add sodium hydroxide to the reaction kettle, and react for 10 hours at a speed of 200r / min and a temperature of 100°C, then cool down to a temperature of 25°C, filter with a microporous membrane, and filter the filtrate Distillation to obtain ethyl benzoylacetate.

[0032] Described microporous membrane is made by following steps:

[0033] After mixing polypropylene, kerosene, and reinforcing fillers uniformly, blend and extrude at a temperature of 40°C. The temperature of the roller is 190°C, the linear speed of the roller is 25m / min, and the speed difference between the upper a...

Embodiment 2

[0040] The preparation method of ethyl benzoyl acetate comprises the steps:

[0041] Step S1: Add carbon tetrachloride and sodium bicarbonate into the reaction kettle, stir at a rotation speed of 150r / min, and a temperature of 25°C, and add ethyl acetoacetate, after stirring for 10 minutes, add benzoyl chloride, The temperature was raised to 60°C, and the reaction was continued for 3 hours;

[0042] Step S2: Add sodium hydroxide to the reaction kettle, and carry out the reaction for 15 hours under the condition of rotating speed of 300r / min and temperature of 100°C, then cool down to a temperature of 25°C, filter with a microporous membrane, and filter the filtrate Distillation to obtain ethyl benzoylacetate.

[0043] Described microporous membrane is made by following steps:

[0044] After mixing polypropylene, kerosene, and reinforcing fillers uniformly, blend and extrude at a temperature of 60°C. The temperature of the roller is 190°C, the linear speed of the roller is 25...

Embodiment 3

[0051] The preparation method of ethyl benzoyl acetate comprises the steps:

[0052] Step S1: Add carbon tetrachloride and sodium bicarbonate into the reaction kettle, stir at a speed of 200r / min, and a temperature of 25°C, and add ethyl acetoacetate, after stirring for 15 minutes, add benzoyl chloride, The temperature was raised to 60°C, and the reaction was continued for 5 hours;

[0053] Step S2: Add sodium hydroxide to the reaction kettle, and carry out the reaction for 15 hours under the condition of the rotating speed of 300r / min and the temperature of 120°C, then cool down to the temperature of 30°C, filter with a microporous membrane, and filter the filtrate Distillation to obtain ethyl benzoylacetate.

[0054] Described microporous membrane is made by following steps:

[0055] After mixing polypropylene, kerosene, and reinforcing fillers evenly, blend and extrude at a temperature of 60°C. The temperature of the roller is 200°C, the linear speed of the roller is 25m / ...

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Abstract

The invention discloses a preparation method of ethyl benzoylacetate, and belongs to the technical field of chemical synthesis. The preparation method comprises the following steps of: adding sodium bicarbonate into carbon tetrachloride, slowly adding ethyl acetoacetate, dropwise adding benzoyl chloride for reaction, adding sodium hydroxide for reaction, and filtering after the reaction is finished to obtain ethyl benzoylacetate. A microporous filter membrane is used in the process of preparing ethyl benzoylacetate. A reinforcing filler is prepared in the process of preparing the microporous filter membrane, and nano silicon dioxide and aniline are treated by the reinforcing filler, so that polyaniline is grafted on the surface of the nano silicon dioxide. Then, the nano silicon dioxide and modified graphene are subjected to ultrasonic treatment to obtain a reinforced substrate. 4-(4-hydroxyphenyl)-2, 3-phthalazine-1-one and epichlorohydrin are subjected to a reaction to prepare epoxy resin, then the epoxy resin and amino groups on the reinforced substrate are cured to prepare a reinforcing filler, the reinforcing filler can enhance the corrosion resistance of the microporous filter membrane, and the microporous filter membrane cannot be corroded after being used for a long time.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of ethyl benzoyl acetate. Background technique [0002] Ethyl benzoyl acetate is an important raw material for the synthesis of color photographic couplers and some pharmaceutical intermediates. The synthesis method usually has the following three methods: ① Use benzaldehyde as the starting material, react with ethyl bromoacetate under the action of metal zinc, and then oxidize the intermediate to obtain: ② Use benzoyl as the raw material under the action of sodium hydride React with ethyl acetoacetate, then treat with concentrated lye to obtain benzoylacetic acid, and then esterify; ③Use ethyl benzoate and ethyl acetoacetate as raw materials to prepare the product under the action of sodium ethoxide. [0003] The existing preparation method of ethyl benzoylacetate needs to be filtered after the reaction is completed, and the surface of the tradit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/343C07C67/48C07C67/56C07C69/738C08J5/18C08L23/12C08L63/00B01D67/00B01D71/46
CPCC07C67/343C07C67/48C07C67/56C08J5/18B01D67/0079B01D71/46C08J2323/12C08J2463/00C07C69/738Y02E60/10
Inventor 汪军汪婷
Owner 江苏巨莱生物医药有限公司
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