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Preparation method of organic intermediate benzoylacetone

A technology of benzoylacetone and benzoylacetone, which is applied in the field of preparation of organic intermediate benzoylacetone, can solve the problems of high raw material price and high cost, and achieves short reaction time, low cost and little environmental pollution Effect

Inactive Publication Date: 2014-05-28
杜承贤
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing synthetic method of benzoylacetone is to adopt acetophenone and ethyl acetate or acetic anhydride, benzoyl chloride and ethyl acetoacetate, benzene and acetic anhydride to be raw material synthetic benzoylacetone, the raw material price that these methods adopt High, the cost of the product is high

Method used

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  • Preparation method of organic intermediate benzoylacetone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] In a four-necked reaction flask equipped with an electric stirrer, a reflux condenser and a thermometer, add 16.8g of diketene, 47.2g of benzene, and 0.4g of a polymerization inhibitor in sequence, start the stirrer, and control the reaction time when the temperature is 85-105°C 5-10h, after stopping the reaction, add 1.5 times the total mass of benzene with hot water at 70-80°C, wash with water, separate the water phase, heat the remaining organic phase to reflux to separate water, decolorize with activated carbon, and filter the organic phase Perform cooling, crystallization and filtration to obtain the benzoylacetone product with a yield of 90.06% and a melting point of 60-61°C.

Embodiment 2

[0015] In a four-necked reaction flask equipped with an electric stirrer, a reflux condenser and a thermometer, add 16.8g of diketene, 59.5g of benzene, and 0.8g of a polymerization inhibitor in sequence, start the stirrer, and control the reaction time when the temperature is 85-105°C 5-10h, after stopping the reaction, add 1.5 times the total mass of benzene with hot water at 70-80°C, wash with water, separate the water phase, heat the remaining organic phase to reflux to separate water, decolorize with activated carbon, and filter the organic phase Perform cooling, crystallization and filtration to obtain the benzoylacetone product with a yield of 90.84% ​​and a melting point of 60-61°C.

Embodiment 3

[0017] In a four-necked reaction flask equipped with an electric stirrer, a reflux condenser and a thermometer, add 16.8g of diketene, 59.5g of benzene, and 1.0g of a polymerization inhibitor in sequence, start the stirrer, and control the reaction time when the temperature is 85-105°C 5-10h, after stopping the reaction, add 1.5 times the total mass of benzene with hot water at 70-80°C, wash with water, separate the water phase, heat the remaining organic phase to reflux to separate water, decolorize with activated carbon, and filter the organic phase Cool down, crystallize and filter to obtain the benzoylacetone product with a yield of 91.32% and a melting point of 60-61°C.

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Abstract

The invention discloses a preparation method of organic intermediate benzoylacetone. The preparation method is characterized in that benzene and diketene are used as raw materials and react in the presence of a polymerization inhibitor so as to prepare the benzoylacetone. The preparation method has the advantages that the benzoylacetone is synthesized, the separation and purification processes are simple, the reaction time is short, the yield of the product reaches above 90%, the product purity is relatively high, the energy consumption is low, the environmental pollution is little, the cost is low, and the preparation method is an ideal technology for realizing industrial production.

Description

technical field [0001] The present invention relates to a kind of preparation method of organic intermediate benzoylacetone. Background technique [0002] Benzoylacetone can be used as chelating extractant, analytical reagent, raw material of spices and intermediate of organic synthesis. Its molecular formula is C 10 h 10 o 2 , molecular weight is 162.19, molecular structure formula: [0003] [0004] Its appearance is colorless crystals with a melting point of 61°C and a boiling point of 261-262°C. The existing synthetic method of benzoylacetone is to adopt acetophenone and ethyl acetate or acetic anhydride, benzoyl chloride and ethyl acetoacetate, benzene and acetic anhydride to be raw material synthetic benzoylacetone, the raw material price that these methods adopt High, the cost of the product is high. Contents of the invention [0005] The purpose of the present invention is in order to overcome above deficiency, a kind of preparation method of benzoylaceton...

Claims

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Application Information

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IPC IPC(8): C07C49/76C07C45/76
CPCC07C45/76C07C49/76
Inventor 杜承贤王树清
Owner 杜承贤