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Method for synthesizing 4,4-dimethoxy-2-butanone

The technology of a dimethoxy group and a synthetic method is applied in the field of fine chemical raw materials, and can solve the problems of expensive methyl formate, inhalation by operators, and troublesome operation, and achieve the effects of low price, easy operation and convenient storage.

Inactive Publication Date: 2011-04-13
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The patent US 5276200 has reported in detail the synthesis of 4,4-dimethoxy-2-butanone with methyl formate as a raw material. The raw material methyl formate in this method is relatively expensive, and the strong base reagent sodium methoxide powder in the process is very easy to mix with the air. Oxygen and moisture reaction, it is not easy to store, and it is easy to be inhaled by the operator, and it will burn the skin when it comes into contact with people, which brings a lot of trouble to the operation

Method used

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  • Method for synthesizing 4,4-dimethoxy-2-butanone

Examples

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Embodiment 1

[0017] (1) In a 1L four-neck flask equipped with a thermometer, a spherical condenser, a stirrer and a nitrogen protection device, add 135g of liquid sodium methoxide, start stirring, heat up to 30°C, and drop 43.5g of acetone and 55.5g of formic acid into it The ethyl ester mixture was added dropwise after 4 hours, and then kept at 30°C for 5 hours to obtain a suspension containing sodium butanone enolate.

[0018] (2) Rotary evaporation was performed on the sodium butanone enolate suspension to remove the solvent and liquid impurities to obtain 53.2 g of a white solid of sodium butanone enolate, and 100 g of methanol was added to form a solution. In another 1L four-necked flask equipped with a thermometer, a spherical condenser, a stirrer and a nitrogen protection device, a mixed solution of 48.3g of concentrated sulfuric acid (98%) and 160g of methanol was added, and the temperature was raised to 25°C. Add the prepared sodium butanone enolate solution dropwise into a four-n...

Embodiment 2

[0021] (1) In a 1L four-neck flask equipped with a thermometer, a spherical condenser, a stirrer and a nitrogen protection device, add 135g of liquid sodium methoxide, start stirring, raise the temperature to 40°C, and drop 43.5g of acetone and 111g of ethyl formate into it The ester mixture was added dropwise after 6 hours, and kept at 40°C for 3 hours to obtain a suspension containing sodium butanone enolate.

[0022] (2) Rotary evaporation was performed on the sodium butanone enolate suspension to remove solvent and liquid impurities to obtain 57.0 g of a white solid of sodium butanone enolate, and 90 g of methanol was added to form a solution. In another 1L four-neck flask equipped with a thermometer, a spherical condenser, a stirrer and a nitrogen protection device, a mixed solution of 77.5g of concentrated sulfuric acid (98%) and 200g of methanol was added, and the temperature was raised to 30°C. Add the prepared sodium butanone enolate solution dropwise into a four-neck...

Embodiment 3

[0025] (1) In a 1L four-neck flask equipped with a thermometer, a spherical condenser, a stirrer and a nitrogen protection device, add 122.7g of liquid sodium methoxide, start stirring, raise the temperature to 50°C, and drop 43.5g of acetone and 166.5g of The mixture of ethyl formate was added dropwise within 7 hours, and then kept at 50°C for 2 hours to obtain a suspension containing sodium butanone enolate.

[0026] (2) Rotary evaporation was performed on the sodium butanone enolate suspension to remove solvent and liquid impurities to obtain 63.3 g of a white solid of sodium butanone enolate, and 80 g of methanol was added to form a solution. In another 1L four-necked flask equipped with a thermometer, a spherical condenser, a stirrer and a nitrogen protection device, a mixed solution of 95.3 g of concentrated sulfuric acid (98%) and 300 g of methanol was added, and the temperature was raised to 35° C. Add the prepared sodium butanone enolate solution dropwise into a four-...

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Abstract

The invention relates to a method for synthesizing a 4,4-dimethoxy-2-butanone fine chemical engineering raw material. The method comprises the following steps of: performing a Claisen condensation reaction of ethyl formate, liquid sodium methoxide, acetone and concentrated sulfuric acid, which serve as raw materials, to prepare butanone sodium enolate, dripping solution of the treated butanone sodium enolate into solution of methanol containing the concentrated sulfuric acid and reacting to obtain a crude product of the 4,4-dimethoxy-2-butanone, and distilling under normal pressure and reduced pressure to obtain the 4,4-dimethoxy-2-butanone. In the invention, the raw materials are cheap, and the method and process are simple, convenient to operate and suitable for large-scale industrial production and have a high industrial application value.

Description

technical field [0001] The invention relates to a preparation method of fine chemical raw material 4,4-dimethoxy-2-butanone. Background technique [0002] 4,4-Dimethoxy-2-butanone is a colorless or light yellow transparent liquid, an important pharmaceutical intermediate of sulfamethazine, widely used in medicine, pesticides, dyes and other fields value. Can synthesize 2-mercapto-4-methylpyrimidine, an important intermediate of medicine and pesticide; synthesize 2-chloro-3-amino-4-methylpyridine, a key intermediate of anti-AIDS drug nevirapine; synthesize ultra-efficient and low-toxic herbicide 5 -Methyl-N-aryl-1,2,4-triazol[1,5-α]pyrimidine-2-sulfonamide; an environmentally friendly water-based coating for electronic equipment shell coating with strong adhesion and stable performance, etc. . [0003] The synthesis of 4,4-dimethoxy-2-butanone in China is still in its infancy, and only a few manufacturers produce it. The production capacity and output are far from meeting ...

Claims

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Application Information

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IPC IPC(8): C07C49/175C07C45/64
Inventor 肖国民姜枫牛磊严间浪陈超明
Owner SOUTHEAST UNIV
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