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One-pot synthesis method of hydroxyacetone

A technology of hydroxyacetone and a synthesis method, which is applied in the preparation of carbonyl compounds, chemical instruments and methods, separation/purification of carbonyl compounds, etc., can solve the problems of high pollution, high cost, complicated process, etc., and achieves less pollution and low cost. , the effect of easy operation

Active Publication Date: 2022-04-12
SINOPHARM CHEM REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to solve the technical problems of high pollution, high cost and complicated process in the existing hydroxyacetone synthesis process, the one-pot synthesis method of hydroxyacetone of the present invention is provided. advantage

Method used

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  • One-pot synthesis method of hydroxyacetone

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Embodiment 1

[0023] The one-pot synthetic method of hydroxyacetone, synthetic reaction route is as follows:

[0024]

[0025] Include the following steps: at 10°C, add 1mol acetone (56.5g), 0.05mol potassium bromide (6g), 0.6mol potassium carbonate (83.0g), 0.03mol tetrabutylammonium bromide (10g) to 300mL In deionized water, mix and stir for 15 minutes to obtain the liquid to be reacted;

[0026] Under stirring, drip hydrogen peroxide (concentration is the aqueous solution of 10wt% hydrogen peroxide, wherein contains hydrogen peroxide 1.05mol) in above-mentioned liquid to be reacted at 10 DEG C, control the rate of addition of hydrogen peroxide to be 0.25-0.3g / min (about 90min drop), the hydrogen peroxide drop is completed, and the temperature is kept at 10°C for 30min; then the temperature is raised to 24°C and the reaction is continued for 60min; after the reaction is completed, solid sodium chloride is added to a saturated state for phase separation, and the organic phase and the in...

Embodiment 2

[0030] The one-pot synthetic method of hydroxyacetone, comprises the following steps: at 15 ℃, with 1mol acetone (56.5g), 0.05mol potassium bromide (6g), 1mol potassium carbonate (76.1g), 0.03mol tetrabutylammonium bromide (10g) was added into 300mL deionized water, mixed and stirred for 15min to obtain the liquid to be reacted;

[0031] Add hydrogen peroxide (concentration is 10wt% hydrogen peroxide aqueous solution, wherein contains hydrogen peroxide 1.03mol) in above-mentioned liquid to be reacted under agitation at 15 ℃, control the dropping speed of hydrogen peroxide to be 0.3-0.35g / min, hydrogen peroxide After the dropwise addition, keep warm at 15°C for 30 minutes; then raise the temperature to 20°C and continue the reaction for 70 minutes; after the reaction is completed, add solid sodium chloride to a saturated state for phase separation, separate the organic phase and the inorganic phase, and use inorganic phase for the inorganic phase. Multiple extractions with wate...

Embodiment 3

[0035] The one-pot synthetic method of hydroxyacetone, comprises the following steps: at 12 ℃, with 1mol acetone (56.5g), 0.05mol potassium bromide (6g), 0.5mol potassium carbonate (69.2g), 0.03mol tetrabutyl bromide Ammonium (10g) was added to 300mL deionized water, mixed and stirred for 15min to obtain the liquid to be reacted;

[0036] Add hydrogen peroxide (the aqueous solution of hydrogen peroxide with a concentration of 10 wt % containing 1 mol of hydrogen peroxide) in the above-mentioned liquid to be reacted under stirring at 12° C., control the rate of addition of hydrogen peroxide to be 0.35-0.45 g / min, the hydrogen peroxide drops After the addition, keep the reaction at 12°C for 30 minutes; then raise the temperature to 23°C and continue the reaction for 60 minutes; after the reaction is completed, add solid sodium chloride to a saturated state for phase separation, separate the organic phase and the inorganic phase, and use anhydrous Multiple extractions with methan...

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Abstract

The invention relates to a one-pot synthesis method of hydroxyacetone, which comprises the following steps: adding acetone, alkali metal bromide, an inorganic acid-binding agent and a phase transfer catalyst into water, and mixing and stirring for at least 10 minutes to obtain a to-be-reacted solution; adding hydrogen peroxide into the to-be-reacted liquid at 10-15 DEG C while stirring, carrying out bromination reaction in the hydrogen peroxide adding process, then carrying out hydrolysis reaction, and in order to enable the reaction to be more complete, raising the temperature to not exceed 25 DEG C and continuing the reaction; and adding salt to a saturated state after the reaction is finished, carrying out phase separation to obtain an organic phase and an inorganic phase, extracting the inorganic phase to obtain an extract liquor, mixing the organic phase with the extract liquor, washing, drying, and desolventizing to finally obtain the hydroxyacetone. The method disclosed by the invention has the advantages of green chemical characteristics, environmental friendliness, simplicity and convenience in operation, low cost, avoidance of the use of an environment-unfriendly lacrimation compound, namely bromoacetone, high efficiency, simplicity and convenience, less pollution and improvement of the working environment.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a one-pot synthesis method of hydroxyacetone. Background technique [0002] Hydroxyacetone, also known as acetol, exists in tobacco leaves, beer, and honey. It is an important intermediate in organic synthesis and can be used to synthesize drugs, spices, and dyes. The molecular structure of hydroxyacetone has important research significance, and its structure reveals the complexity between adjacent energy levels of molecular complexes containing carbon-oxygen bonds. Hydroxyacetone is an important initial material for the synthesis of many compounds, such as acetals and ketals, and is also an important raw material for the synthesis of digestive system drugs cimetidine, quinolone antibacterial drugs, and antipyretic and analgesic drugs such as aspirin acetonate . [0003] The preparation method of hydroxyacetone in the prior art roughly has the following several kinds...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/17C07C45/64C07C45/78C07C45/80C07C45/81
CPCY02P20/584
Inventor 郭建国吕文华吴孝兰贾自自
Owner SINOPHARM CHEM REAGENT
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