Process for synthesizing 2-hydroxy-2-methyl-1-phenyl-1-propyl ketone

A synthesis process, the technology of acetone, applied in the preparation of carbon-based compounds, the preparation of organic compounds, organic chemistry, etc., can solve the problems of increased environmental pollution and low product yield, and achieve reasonable synthesis process and high product yield High and low environmental pollution effect

Inactive Publication Date: 2012-01-04
LIANYUNGANG SHENGNAN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The defect of this synthesis process is that the synthesis process will produce sulfur dioxide, sodium bromide and other substances, which will increase environmental pollution and lower product yield.

Method used

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  • Process for synthesizing 2-hydroxy-2-methyl-1-phenyl-1-propyl ketone
  • Process for synthesizing 2-hydroxy-2-methyl-1-phenyl-1-propyl ketone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1, a kind of synthetic technique of 2-hydroxyl-2-methyl-1-phenyl-1-propyl ketone, its steps are as follows:

[0028] ⑴Acylation: Put isobutyric acid into the reaction kettle, raise the temperature to 45°C, add phosphorus trichloride, keep it at 48°C for at least 4 hours, remove the inorganic layer to obtain isobutyryl chloride; the raw material isobutyric acid and trichloride The weight ratio of phosphorus is 10:6.8;

[0029] (2) Friedel-Crafts reaction: Add benzene and catalyst aluminum trichloride to the reaction kettle, after cooling down to 5°C, add isobutyryl chloride dropwise, the weight ratio of benzene, aluminum trichloride and isobutyryl chloride is 9:5.0:4.0 , at 10°C for at least 2.5 hours to obtain a complex of 2-methyl-1-phenyl-1-propyl ketone and aluminum trichloride;

[0030] (3) Hydrolysis reaction: add the complex to an appropriate amount of dilute hydrochloric acid with a mass concentration of 1.5%, stir and separate layers, remove the aque...

Embodiment 2

[0034] Embodiment 2, a kind of synthetic technique of 2-hydroxyl-2-methyl-1-phenyl-1-propyl ketone, its steps are as follows:

[0035] ⑴Acylation: Put isobutyric acid into the reaction kettle, raise the temperature to 50°C, add phosphorus trichloride, keep it at 52°C for at least 4 hours, remove the inorganic layer to obtain isobutyryl chloride; the raw material isobutyric acid and trichloride The weight ratio of phosphorus is 10:7.2;

[0036] (2) Friedel-Crafts reaction: Add benzene and catalyst aluminum trichloride to the reaction kettle, after cooling down to 10°C, add isobutyryl chloride dropwise, the weight ratio of benzene, aluminum trichloride and isobutyryl chloride is 9:5.4:4.2 , at 15°C for at least 2.5 hours to obtain a complex of 2-methyl-1-phenyl-1-propyl ketone and aluminum trichloride;

[0037] (3) Hydrolysis reaction: Add the complex to an appropriate amount of dilute hydrochloric acid with a mass concentration of 2.5%, stir and separate layers, remove the aqu...

Embodiment 3

[0041] Embodiment 3, a kind of synthetic technique of 2-hydroxyl-2-methyl-1-phenyl-1-propyl ketone, its steps are as follows:

[0042] ⑴Acylation: Put isobutyric acid into the reaction kettle, raise the temperature to 47°C, add phosphorus trichloride, keep it at 50°C for at least 4 hours, remove the inorganic layer to obtain isobutyryl chloride; the raw material isobutyryl chloride and trichloride The weight ratio of phosphorus is 10:7;

[0043] (2) Friedel-Crafts reaction: Add benzene and catalyst aluminum trichloride to the reaction kettle, after cooling down to 8°C, add isobutyryl chloride dropwise, the weight ratio of benzene, aluminum trichloride and isobutyryl chloride is 9:5.2:4.1 , at 12°C for at least 2.5 hours to obtain a complex of 2-methyl-1-phenyl-1-propyl ketone and aluminum trichloride;

[0044] (3) Hydrolysis reaction: add the complex to an appropriate amount of dilute hydrochloric acid with a mass concentration of 2%, stir and separate layers, remove the aque...

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Abstract

The invention relates to a process for synthesizing 2-hydroxy-2-methyl-1-phenyl-1-propyl ketone, which is characterized by comprising the following steps of: obtaining a crude product of 2-hydroxy-2-methyl-1-phenyl-1-propyl ketone by using isobutyric acid as raw material via acylation, Friedel-Crafts and alkaline hydrolysis reaction; then finely steaming to obtain a finished product of the 2-hydroxy-2-methyl-1-phenyl-1-propyl ketone. The synthesis process provided by the invention is more reasonable, no sulfur dioxide gas is released in the production process, the generated sodium chloride has less environment pollution, and the product yield is high.

Description

technical field [0001] The invention relates to a synthesis process of 2-hydroxy-2-methyl-1-phenyl-1-propyl ketone. Background technique [0002] The synthesis process of 2-hydroxy-2-methyl-1-phenyl-1-propyl ketone in the prior art is mainly: isobutyric acid is chlorinated by thionyl chloride, isobutyryl chloride and benzoylation to generate an intermediate Methylpropiophenone, the latter is hydrolyzed by bromination to generate n-hydroxy-a-methylpropiophenone. The defect of this synthesis process is that the synthesis process will produce substances such as sulfur dioxide and sodium bromide, which will increase environmental pollution and the product yield is low. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide a 2-hydroxy-2-methyl-1-phenyl-1-propyl ketone with a more reasonable process, safety and environmental protection, and a higher yield for the deficiencies of the prior art synthesis process. [0004] ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/82C07C45/64
Inventor 周东
Owner LIANYUNGANG SHENGNAN CHEM
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