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A kind of continuous production device and method of 2,4-difluoro-3-methoxybenzoic acid

A technology of methoxybenzoic acid and m-difluorobenzene, which is applied in the field of continuous production equipment of 2,4-difluoro-3-methoxybenzoic acid, and can solve the problems affecting the continuity of reaction and the reduction of production efficiency

Active Publication Date: 2020-12-15
TAIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The main problem of the above synthesis method is that the reaction temperature in the first step and the last step is between -80°C~-75°C, and the temperature in the middle reaction process is between room temperature and 45°C. Due to the huge difference in the reaction temperature, this The synthetic method is only suitable for intermittent production, which affects the continuity of the reaction and greatly reduces the production efficiency

Method used

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  • A kind of continuous production device and method of 2,4-difluoro-3-methoxybenzoic acid
  • A kind of continuous production device and method of 2,4-difluoro-3-methoxybenzoic acid
  • A kind of continuous production device and method of 2,4-difluoro-3-methoxybenzoic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0088] (1) m-difluorobenzene solution and organolithium are sampled in module one of the first temperature zone, and boric acid ester is sampled in module two, and borated reaction solution is obtained after quenching separation module one quenching and separating;

[0089] (2) The boration reaction liquid enters the module three of the second temperature zone to react with the oxidizing agent to obtain the oxidation reaction liquid;

[0090] (3) The methylation reagent is injected into module four, and undergoes a methylation reaction with the oxidation reaction solution to obtain a methylation reaction solution;

[0091] (4) The methylation reaction liquid passes through the quenching separation module two and the obtained oil phase enters the module five of the third temperature zone to react with organic lithium, and the CO 2 Sampling is injected in module six, and the carboxylation reaction is reversed; quenching agent water is injected in quenching / separation module thre...

Embodiment 2

[0094] The steps in Example 1 were used to produce 2,4-difluoro-3-methoxybenzoic acid. The types of raw materials used, the sampling rate, the temperature in each temperature zone and the total production time are shown in Table 1.

Embodiment 3

[0096] The steps in Example 1 were used to produce 2,4-difluoro-3-methoxybenzoic acid. The types of raw materials used, the sampling rate, the temperature in each temperature zone and the total production time are shown in Table 1.

[0097] Table 1 The types of raw materials used in Examples 1 to 3, the sampling rate, the temperature of the warm zone and the total production time

[0098]

[0099]

[0100] Note: The molar ratio of raw materials in Examples 1 to 3: m-difluorobenzene: trimethyl borate: n-butyl lithium: hydrogen peroxide: dimethyl sulfate: n-butyl lithium: CO 2 =1.0:1.0:1.0:1.0:1.0:1.0:1.0.

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Abstract

The invention provides a continuous production device and method for 2,4-difluoro-3-methoxybenzoic acid, belonging to the technical field of pharmaceutical intermediates. In the present invention, by dividing the production device into three temperature zones, it can cooperate with the temperature change in the synthesis process of 2,4-difluoro-3-methoxybenzoic acid, and avoid the production of discontinuous; the production device of the present invention includes nine modules, and three quenching separations in the production process, hydrogen extraction reaction, borylation reaction, oxidation reaction, methylation reaction and carboxylation reaction and production process are respectively in different Carry out in the module, can realize the continuous production of 2,4-difluoro-3-methoxybenzoic acid; The present invention adopts microchannel reactor to replace traditional reactor, has increased the heat exchange of reaction process, has shortened reaction time , improving production efficiency and reducing reaction energy consumption.

Description

technical field [0001] The invention relates to the technical field of production of pharmaceutical intermediates, in particular to a continuous production device and method for 2,4-difluoro-3-methoxybenzoic acid. Background technique [0002] Quinolones are a new type of synthetic high-efficiency broad-spectrum antibacterial drugs, which mainly act on Gram-negative bacteria, have weak effects on Gram-positive bacteria, and have good antibacterial effects on other antibiotic-resistant bacteria. Although quinolones have been widely used in the treatment of a variety of bacterial infections, their irrational use has led to bacterial resistance becoming a serious problem. Studies have shown that most methicillin-resistant Staphylococcus aureus (MRSA) Existing quinolones are drug-resistant, so research on new powerful quinolones has never stopped. [0003] With the deepening of research, new quinolone antibacterial drugs are constantly emerging, and the research on the synthesi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J19/00C07C51/15C07C65/21C07C37/01C07C39/27C07C41/16C07C43/225C07F5/02
CPCB01J19/0046B01J19/0093C07C37/01C07C41/16C07C51/15C07F5/025C07C65/21C07C39/27C07C43/225
Inventor 韩得满李嵘嵘吴佳春
Owner TAIZHOU UNIV