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A kind of 1-phenyl-1-propanone synthetic method

A synthesis method, acetone technology, applied in the direction of condensation preparation of carbonyl compounds, aluminum chloride, aluminum halide, etc., can solve the problems of non-recycling of waste water, environmental pollution, etc., and achieve the effect of low cost, significant economic benefits, and mild reaction conditions

Inactive Publication Date: 2015-08-19
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] Wu Yinwen of Hebei Medical University adopted the synthesis method of Wieliam T Read, using benzene and propionyl chloride as raw materials, using AlCl3 as a catalyst, and After the reaction, the steam distillation was changed to an extraction operation. Compared with the original process, although the yield increased from 84% to 88.6%, the reaction was carried out at 50°C, which easily produced an emulsified layer, and the waste water was not recycled. easy to cause environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Control the internal temperature at 20~25°C, slowly add 195g (2.5mol) of benzene and 120.0g (0.9mol) of aluminum trichloride to the three-necked flask in sequence, and after stirring for 1.0 h, slowly add 74g (0.80mol) of ) Propionyl chloride, 2 h drop;

[0030] (2) Add 14.7g (0.11mol) of aluminum trichloride to step (1), stir for 0.5h, then slowly add 18.5g (0.20mol) of propionyl chloride dropwise, raise the temperature to 35°C, and keep the temperature for 2h. After the reaction is completed, ;

[0031] (3) Cool the reaction solution in step 2) to 25°C, add it dropwise into an aqueous solution for hydrolysis, let it stand, and separate layers. The upper layer is a milky white organic phase, and the lower layer is a light yellow aqueous phase;

[0032] (4) The organic phase of the upper layer in step (2) is distilled under normal pressure to separate benzene; after vacuum distillation, and then under vacuum distillation at 20mmHg, the temperat...

Embodiment 2

[0035] (1) Control the internal temperature at 20~25°C, slowly add 195g (2.5mol) of benzene and 120g (0.9mol) of aluminum trichloride to the three-necked flask in sequence, and after stirring for 1.0 h, slowly add 74g (0.80mol) dropwise Propionyl chloride, drop over 2 h;

[0036] (2) Add 17.3g (0.13mol) of aluminum trichloride to step (1), stir for 0.5h, then slowly add the remaining 18.5g (0.20mol) of propionyl chloride dropwise, raise the temperature to 35°C, and react for 2h;

[0037] (3) The reaction solution in step 2) was cooled to 25°C, added dropwise into an aqueous solution for hydrolysis, left to stand, and separated into layers. The upper layer was a milky white organic phase, and the lower layer was a light yellow aqueous phase;

[0038] (4) The organic phase of the upper layer in step (2) is distilled under normal pressure to separate benzene; after vacuum distillation, and then under vacuum distillation at 20mmHg, the temperature is controlled t...

Embodiment 3

[0041] (1) Control the internal temperature at 20~25°C, slowly add 195g (2.5mol) of benzene and 120g (0.9mol) of aluminum trichloride to the three-necked flask in sequence, and after stirring for 1.0 h, slowly add 78.6g (0.85mol) ) Propionyl chloride, 2 h drop;

[0042] (2) Add 20.0g (0.15mol) of aluminum trichloride to step (1), stir for 0.5h, then slowly add the remaining 18.5g (0.20mol) of propionyl chloride dropwise, raise the temperature to 35°C, and react for 2h;

[0043] (3) The reaction solution in step 2) was cooled to 25°C, added dropwise into an aqueous solution for hydrolysis, left to stand, and separated into layers. The upper layer was a milky white organic phase, and the lower layer was a light yellow aqueous phase;

[0044] (4) The organic phase of the upper layer in step (2) is distilled under normal pressure to separate benzene; after vacuum distillation, and then under vacuum distillation at 20mmHg, the temperature is controlled to 180-185°C, an...

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Abstract

The invention relates to a synthetic method for 1-phenyl-1-acetone. The synthetic method comprises the following steps: with benzene as a raw material and a solvent, adding propionyl chloride and AlCl3 in two steps at a temperature of 25 to 35 DEG C under the catalysis conditions of AlCl3; and carrying out a Friedel-Crafts acylation reaction to synthesize 1-phenyl-1-acetone. The synthetic method has the advantages of simple process, low cost, mild reaction conditions, product yield of more than 96%, product purity of 99.9%, maximum utilization of waste liquid for preparation of AlCl3.6H2O, no ecological environment risks, substantial economic benefits and suitability for large scale industrial production.

Description

technical field [0001] The invention relates to a synthesis method of 1-phenyl-1-acetone, specifically a green synthesis method for synthesizing 1-phenyl-1-acetone by using benzene and propionyl chloride as raw materials through Friedel-Crafts acylation reaction, which belongs to chemical synthesis field. Background technique [0002] 1-Phenyl-1-propanone is used as an intermediate of drugs methine and cholesterol as well as a fragrance fixative. At present, the traditional process of industrial production of propiophenone in China, one is to use iron and its oxides as catalysts, and condense benzoic acid and propionic acid to obtain 1-phenyl-1-acetone, which has many by-products, low yield and complicated separation technology; The 2nd, Lewis acid is used as catalyst, and benzene, propionyl chloride are directly condensed to obtain propiophenone, and catalyst excess is 0.1-0.2mol, and reaction temperature is high, and yield is low, easily produces a large amount of emulsif...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/76C07C45/46C01F7/56
CPCC01F7/56C07C45/46C07C49/76
Inventor 李德江张义军刘义稳陈义兴王艳玲龚大春
Owner CHINA THREE GORGES UNIV