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Microchannel reaction method of 4-chloroethyl acetoacetate and device

A technology of ethyl chloroacetoacetate and microchannel reaction, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and preparation of ketene/polyketene, etc., which can solve the problems of difficult disposal of solid waste, increased production costs, and by-products increase and other problems, to achieve the effect of easy control of reaction temperature, high production capacity and sufficient reaction

Active Publication Date: 2019-03-22
ANHUI JINGHE IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a microchannel reaction of ethyl 4-chloroacetoacetate in order to solve the problems of increased by-products, increased production costs, low yield and difficult disposal of solid waste in the production of the existing diketene method. Method and device

Method used

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  • Microchannel reaction method of 4-chloroethyl acetoacetate and device

Examples

Experimental program
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Effect test

example 1

[0018] A kind of microchannel reaction method of ethyl 4-chloroacetoacetate, concrete implementation steps are as follows:

[0019] 1. Open the refrigerant valves of the 1st, 2nd, 3rd, and 4th reaction modules of the microchannel reactor, close the refrigerant valve of the 5th reaction module, control the refrigeration temperature at 3 ° C, diketene and dichloromethane according to the volume ratio of 2:1 Mix in the diketene tank first, then enter the first reaction module of the microchannel reactor at a flow rate of 10mL / min after mixing, and simultaneously pass chlorine gas with a pressure of 0.25Mpa and a flow rate of 1500mL / min into the first reaction module of the microchannel reactor. Chlorination reaction;

[0020] 2. When the chlorination reaction solution from the fourth reaction module reaches the fifth reaction module, add absolute ethanol to the fifth reaction module, control the flow rate at 6mL / min, and control the reaction temperature of the fifth reaction modu...

example 2

[0023] 1. The refrigerant valve of the 1st, 2, 3, 4 reaction modules of the microchannel reactor is opened, the refrigerant valve of the 5th reaction module is closed, the refrigeration temperature is controlled at -8 ℃, diketene and dichloromethane are according to volume ratio 3: 1 Mix in a diketene tank first, then enter the first reaction module of the microchannel reactor at a flow rate of 15mL / min after mixing, and simultaneously pass chlorine gas with a pressure of 0.28Mpa and a flow rate of 3000mL / min into the first reaction module of the microchannel reactor carry out chlorination reaction;

[0024] 2. When the chlorination reaction solution from the fourth reaction module reaches the fifth reaction module, add absolute ethanol to the fifth reaction module, control the flow rate at 8mL / min, and control the reaction temperature of the fifth reaction module at 60°C;

[0025] 3. The esterification reaction solution from the fifth reaction module is firstly distilled (at ...

example 3

[0027] 1. Open the refrigerant valves of the 1st, 2nd, 3rd and 4th reaction modules of the microchannel reactor, close the refrigerant valves of the 5th reaction module, and control the refrigeration temperature at -15°C. Diketene and methylene chloride are in a volume ratio of 3.5: 1 Mix in the diketene tank first, then enter the first reaction module of the microchannel reactor at a flow rate of 20mL / min after mixing, and simultaneously pass chlorine gas with a pressure of 0.30Mpa and a flow rate of 4000mL / min into the first reaction module of the microchannel reactor carry out chlorination reaction;

[0028] 2. When the chlorination reaction solution from the fourth reaction module reaches the fifth reaction module, add absolute ethanol to the fifth reaction module, control the flow rate at 10mL / min, and control the reaction temperature of the fifth reaction module at 50°C;

[0029] 3. The esterification reaction solution from the fifth reaction module is firstly distilled ...

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Abstract

The invention relates to a microchannel reaction method of 4-chloroethyl acetoacetate and a device. The method is characterized by comprising the following steps: 1. mixing a ketene dimer and dichloromethane according to the volume ratio of (2 to 3.6): 1 in a ketene dimer tank, then, carrying out charging from a first reaction module at a flow velocity of 10mL / min to 25mL / min, introducing chlorinegas to the first reaction module, and controlling the chlorine gas pressure to 0.25MPa to 0.3MPa, the flow velocity to 1,500mL / min to 7,500mL / min and the reaction temperature to -18 DEG C to 3 DEG C;2. introducing anhydrous ethanol to a fifth reaction module when a chlorination reaction solution enters the fifth reaction module, and controlling the flow velocity to 6mL / min to 10mL / min and the reaction temperature to 40 DEG C to 70 DEG C; 3. subjecting an esterification reaction solution come from the fifth reaction module to distillation and rectification sequentially, thereby obtaining the4-chloroethyl acetoacetate. The method and the device have the advantages that both a chlorination reaction and an esterification reaction are carried out in a microchannel reactor, the reaction speedis high, the production capacity is large, and the reaction temperature is easier to control; chlorine gas is not dissolved in an organic solvent, so that the reaction is more thorough, and the efficiency is higher; a stabilizer is not required to be added, so that the difficulty of subsequent solid waste treatment is lowered; the residence time of materials during reaction is short, and thus, the occurrence of side reactions is reduced.

Description

technical field [0001] The invention belongs to the technical field of chemical production and relates to a microchannel reaction method and device for ethyl 4-chloroacetoacetate. Background technique [0002] 4-Chloroacetoacetic acid ethyl ester is a colorless liquid with a density of 1.218. Its English name is 4-Chloroacetoacetic acid ethyl ester, and its CAS is 638-07-3. It is the key intermediate of the new generation of nootropic drug oxiracetam. Oxiracetam is a nootropic that acts on the cholinergic brainstem reticular structure. It increases the level of ATP in the brain by stimulating the conversion of adenosine diphosphate to adenosine triphosphate (ATP), accelerates the metabolism of brain phospholipids, stimulates Synthesis of brain ribonic acid and protein, enhance the tolerance of cerebral cortex to hypoxia, reduce cerebrovascular resistance, restore cerebral blood flow, prevent secondary lesions, have a certain effect on strengthening memory and restoring brain...

Claims

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Application Information

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IPC IPC(8): C07C69/72C07C67/46C07C67/54C07D305/12
CPCC07C67/46C07C67/54C07D305/12C07C69/72
Inventor 施以军石剑朱敏
Owner ANHUI JINGHE IND
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