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Method for preparing 3,3-dimethoxy-2-butanone

A technology of dimethoxy and dibutyl ketone, which is applied in the field of preparation of 3,3-dimethoxy-2-butanone, can solve the problems of increasing pollution of three wastes and achieve the effect of reducing pollution of three wastes and simple preparation method

Inactive Publication Date: 2017-11-24
太仓市茜泾化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

As a result, a large amount of aqueous waste methanol will be produced during the post-processing of the product, increasing the pollution of the three wastes

Method used

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  • Method for preparing 3,3-dimethoxy-2-butanone
  • Method for preparing 3,3-dimethoxy-2-butanone

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Embodiment 1

[0023] This embodiment provides a preparation method of 3,3-dimethoxy-2-butanone, the preparation method is as follows:

[0024] Add 2,3-dibutanone (47.3g, 0.55mol) and p-toluenesulfonic acid (0.06g) into the reaction flask, start stirring, slowly drop trimethyl orthoformate (64.13g, 0.605mol) and The mixture of p-toluenesulfonic acid (0.13g) was added dropwise for 2 hours. The reaction was continued for 7 hours at 20° C., and the reaction ended. Potassium carbonate (1 g) was then added for neutralization, stirred for 1 hour, and then distilled under reduced pressure at 100 mmHg to obtain a crude product. Distill once more at 90°C / 200mbar to obtain the product. Yield: 80%.

Embodiment 2

[0026] This embodiment provides a preparation method of 3,3-dimethoxy-2-butanone, the preparation method is as follows:

[0027] Add 2,3-dibutanone (47.3g, 0.55mol) into the reaction flask, start stirring, slowly add trimethyl orthoformate (64.13g, 0.605mol) and p-toluenesulfonic acid (0.19g) dropwise at 15°C and mix solution, the dropwise addition time is 1.5 hours. The reaction was continued for 7 hours at 15° C., and the reaction was completed. Potassium carbonate (1 g) was then added for neutralization, stirred for 1 hour, and then distilled under reduced pressure at 100 mmHg to obtain a crude product. Distill once more at 90°C / 200mbar to obtain the product. Yield: 83%.

Embodiment 3

[0029] This embodiment provides a preparation method of 3,3-dimethoxy-2-butanone, the preparation method is as follows:

[0030] Add 2,3-dibutanone (47.3g, 0.55mol) and p-toluenesulfonic acid (0.09g) into the reaction flask, start stirring, slowly drop trimethyl orthoformate (87.55g, 0.825mol) and The mixture of p-toluenesulfonic acid (0.21g) was added within two hours. The reaction was continued for 7 hours at 25° C., and the reaction was completed. Potassium carbonate (1.5 g) was then added for neutralization, stirred for 1 hour, and then distilled under reduced pressure at 100 mmHg to obtain a crude product. Distill once more at 90°C / 200mbar to obtain the product. Yield: 81%.

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Abstract

The invention relates to a method for preparing 3,3-dimethoxy-2-butanone. The method comprises the following step: enabling trimethyl orthoformate and 2,3-dibutanone to react in the presence of a catalyst, thereby obtaining 3,3-dimethoxy-2-butanone. According to the method provided by the invention, trimethyl orthoformate and 2,3-dibutanone are adopted as raw materials, products include 3,3-dimethoxy-2-butanone and methyl formate, and the generated methyl formate can be used as a solvent in a system and only needs to be removed through vacuum steaming. Compared with a conventional method that methanol and 2,3-dibutanone are adopted as raw materials, the method is low in waste pollution and simple in preparation, and the yield can be up to 80% or higher.

Description

technical field [0001] The invention relates to a preparation method of 3,3-dimethoxy-2-butanone. Background technique [0002] The CAS number of 3,3-dimethoxy-2-butanone is 21983-72-2. At present, the preparation of 3,3-dimethoxy-2-butanone is usually 2,3-dibutanone and methanol as a raw material to prepare, such as the preparation method of 3,3-dimethoxy-2-butanone disclosed in U.S. Patent US2401336 is that 2,3-dimethoxy-2-butanone reacts with methanol in the presence of an acidic catalyst to prepare 3,3-Dimethoxy-2-butanone, the reaction equation is as follows [0003] [0004] Because the reaction is reversible, considering that the reaction is an equilibrium reaction, a portion of water is generated, and for the reaction to proceed to the right, at least five times the weight of methyl alcohol is added. As a result, a large amount of aqueous waste methanol will be produced in the post-treatment process of the product, which increases the pollution of the three wast...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/64C07C49/175
CPCC07C45/64
Inventor 吴健明
Owner 太仓市茜泾化工有限公司