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Synthesis method of 4,4-dimethoxy-2-butanone

A technology of dimethoxy and synthesis method, which is applied in the field of synthesis of 4,4-dimethoxy-2-butanone, can solve problems such as difficulty in amplification, achieves promoting mixing, avoiding heat storage, improving reaction rate and Pure quality effects

Pending Publication Date: 2021-11-05
南京硕达生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the intense heat release during the reaction process, it is currently difficult to scale up in industry

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A kind of synthetic method of 4,4-dimethoxy-2-butanone, it is characterized in that: operating steps are as follows in sequence:

[0019] S1: Solution preparation: add metal sodium to methanol solution to prepare sodium methoxide solution as solution 1, the mass ratio of methanol to metal sodium is 7:1, and the temperature is controlled at 0-10°C during the configuration process; acetone and ethyl formate Mixed as solution 2, the mass ratio of ethyl formate and acetone is 1:3; concentrated sulfuric acid is directly fed as raw material solution 3; the molar ratio of sodium methylate to acetone is 1:1.1; the molar ratio of the amount of concentrated sulfuric acid to the amount of acetone is 3:1.

[0020] S2: Build the reactor: use a tangential flow reactor for the synthesis reaction, the total volume of the reactor is 5L, use a diaphragm pump to transport the raw material liquid, and the inlet ports of the diaphragm pumps 1, 2 and 3 are in phase with the raw material liqu...

Embodiment 2

[0025] A kind of synthetic method of 4,4-dimethoxy-2-butanone, it is characterized in that: operating steps are as follows in sequence:

[0026] S1: Solution preparation: Add metal sodium to methanol solution to prepare sodium methoxide solution as solution 1, the mass ratio of methanol to metal sodium is 8:1, and the temperature is controlled at 0-10°C during the configuration process; acetone and ethyl formate Mixed as solution 2, the mass ratio of ethyl formate and acetone is 1:3; concentrated sulfuric acid is directly fed as raw material solution 3; the molar ratio of sodium methylate to acetone is 1:1.2; the molar ratio of the amount of concentrated sulfuric acid to the amount of acetone is 3:1.

[0027] S2: Build the reactor: use a tangential flow reactor for the synthesis reaction, the total volume of the reactor is 5L, use a diaphragm pump to transport the raw material liquid, and the inlet ports of the diaphragm pumps 1, 2 and 3 are in phase with the raw material liqu...

Embodiment 3

[0032] A kind of synthetic method of 4,4-dimethoxy-2-butanone, it is characterized in that: operating steps are as follows in sequence:

[0033] S1: Solution preparation: add metal sodium to methanol solution to prepare sodium methoxide solution as solution 1, the mass ratio of methanol to metal sodium is 7:1, and the temperature is controlled at 0-10°C during the configuration process; acetone and ethyl formate Mixed as solution 2, the mass ratio of ethyl formate and acetone is 1:4; concentrated sulfuric acid is directly fed as raw material solution 3; the molar ratio of sodium methylate to acetone is 1:1.1; the molar ratio of the amount of concentrated sulfuric acid to the amount of acetone is 4:1.

[0034] S2: Build the reactor: use a tangential flow reactor for the synthesis reaction, the total volume of the reactor is 5L, use a diaphragm pump to transport the raw material liquid, and the inlet ports of the diaphragm pumps 1, 2 and 3 are in phase with the raw material liqu...

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Abstract

The invention discloses a synthesis method of 4,4-dimethoxy-2-butanone, wherein the synthesis method comprises the following steps: S1, preparing raw material liquids, wherein the raw material liquid 1 is a sodium methoxide solution, the raw material liquid 2 is a mixed solution of acetone and ethyl formate, and the raw material liquid 3 is concentrated sulfuric acid; S2, building a reactor: carrying out a synthesis reaction by adopting a tangential flow reactor, wherein the total volume of the reactor is 5 L; S3, preparing 4,4-dimethoxy-2-butanone: starting the tangential flow reactor and a diaphragm pump to carry out a synthetic reaction; and S4, post-treatment: neutralizing the solution, filtering, carrying out atmospheric distillation, and carrying out reduced pressure distillation to obtain a 4,4-dimethoxy-2-butanone product. According to the invention, a continuous flow mode is adopted for reaction, so that heat storage of a reaction kettle is effectively avoided, and the operation safety of each part is improved. And meanwhile, a microreactor is adopted to promote mixing of reactions in all steps, so that the reaction rate and the pure product quality are improved, the reaction time is shortened, and the production efficiency of enterprises is improved.

Description

technical field [0001] The invention relates to the field of pesticide preparation, in particular to a synthesis method of 4,4-dimethoxy-2-butanone. Background technique [0002] 4,4-Dimethoxy-2-butanone is an important pharmaceutical intermediate of sulfamethazine, which is widely used in medicine, pesticides, dyes and other fields. At present, the synthesis of 4,4-dimethoxy-2-butanone in China is still in its infancy, and the production capacity and output are far from meeting the actual domestic production needs, seriously affecting the development of its downstream products and the promotion of new production technologies . At present, most reports use methyl formate as raw material to synthesize 4,4-dimethoxy-2-butanone. Methyl formate and acetone are used as raw materials to prepare sodium butanone enolate through Claisen ester condensation reaction under the action of a strong alkali reagent, and then sodium butanone enolate undergoes neutralization reaction and add...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/68C07C49/24C07C45/64C07C45/82C07C49/175B01D3/00
CPCC07C45/68C07C45/64C07C45/82B01D3/009C07C49/24C07C49/175
Inventor 席亚男张俊
Owner 南京硕达生物科技有限公司
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