Preparation method of florfenicol

A technology of florfenicol and auxiliary devices, which is applied in the field of preparation of florfenicol, can solve the problems of no targeted discharge method of hydrogen gas, lack of yield of florfenicol, etc., to facilitate mass processing, convenient and simple operation Extensive, easy-to-operate effect

Pending Publication Date: 2021-08-13
HUBEI ZHONGMU ANDA PHARMACEUTICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The first purpose of the present invention is to solve the problem of lack of high yield and easy operation in the preparation of florfenicol in the prior art, and the problem of other waste less preparation routes, and the second is to solve the problem of the non-targeted discharge means of hydrogen caused by the use of KBH4 The problem

Method used

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  • Preparation method of florfenicol
  • Preparation method of florfenicol
  • Preparation method of florfenicol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] The invention claims to protect a feeding auxiliary device for preparing florfenicol, which is characterized in that it includes a reduction reaction kettle 1, an air inlet part 2, an air outlet part 3, a funnel part 4, a crossbar part 5, an ultrasonic device 6, and a left support Part 7, right support part 8.

[0043] The reduction reaction kettle 1 is equipped with an upper port 11, an air inlet 12, an air outlet 13, a feeding port 14, and a stirrer 15, and the upper port 11, the air inlet 12, the air outlet 13, and the feeding port 14 are respectively adapted to the upper Port cover 111, air inlet cover 121, air outlet cover 131, and feed port cover 141; the upper port 11 is located directly above the reduction reaction kettle, and the air inlet 12 and the feed port 14 are located on the inclined surface on the right side of the upper port 11 , the gas outlet 13 is located on the inclined surface on the left side of the upper port 11, and the axis of the feeding port...

Embodiment 2

[0054] (1) Installation and test run steps: remove the upper cover, air inlet cover, and air outlet cover of the reduction reaction kettle, install the air inlet plug and the air outlet plug respectively, and install the air inlet glass tube (23) and Air outlet glass tube (33), and connect the air intake pipe (21), air intake pump (22) and air outlet pipe (31), air outlet pump (32) respectively, cover the upper mouth cover (111), use the air inlet part with 1.4 -1.6L / min speed into the nitrogen, and use the gas outlet to export the gas at the same speed, open and close the upper port repeatedly and monitor until the opening and closing will not cause significant changes in air pressure; this step is to ensure the installation, and the second is to ensure the air flow smooth.

[0055] (2) Steps of installing the funnel part: install the left support part and the right support part at the front and back of the funnel part, remove the feeding port cover and replace it with a seal...

Embodiment 3

[0063] (1) Installation and test run steps: remove the upper cover, air inlet cover, and air outlet cover of the reduction reaction kettle, install the air inlet plug and the air outlet plug respectively, and install the air inlet glass tube (23) and Air outlet glass tube (33), and connect the air intake pipe (21), air intake pump (22) and air outlet pipe (31), air outlet pump (32) respectively, cover the upper mouth cover (111), use the air inlet part with 1.4 -1.6L / min speed into the nitrogen, and use the gas outlet to export the gas at the same speed, open and close the upper port repeatedly and monitor until the opening and closing will not cause a significant change in the air pressure;

[0064] (2) Steps of installing the funnel part: install the left support part and the right support part at the front and back of the funnel part, remove the feeding port cover and replace it with a sealing ring, and the sealing ring is tightly set on the feeding port, so that the ring pa...

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Abstract

A preparation method of florfenicol comprises the following steps of: reacting D-ethyl ester with methanol and potassium borohydride to obtain a first-step product; obtaining a second-step product, namely an intermediate cyclization compound, from the first-step product under the action of dichloroacetonitrile and glacial acetic acid, preparing a third-step product, namely an Ishikawa fluorination reagent, from dichloromethane, diethylamine and hexafluoropropylene, reacting the second-step product with the third-step product by taking the dichloromethane as a solvent to obtain a fourth-step product, namely a fluorination reaction solution, and transferring the fourth-step product into a hydrolysis kettle; adding water and sodium acetate into the fourth-step product in the hydrolysis kettle, heating and distilling to evaporate dichloromethane, adding the final crystallization mother liquor of the previous batch after evaporation, heating for reaction, discharging most of isopropanol and water, cooling, and centrifugally separating to obtain crude florfenicol; and refining the crude florfenicol to obtain a pure product, and recycling crystallization mother liquor. A feeding auxiliary device is further arranged and used for effectively adding potassium borohydride in the first step and treating hydrogen in the dissolving process.

Description

technical field [0001] The invention relates to the technical field of pharmacy and chemical industry, in particular to a preparation method of florfenicol. Background technique [0002] Florfenicol, also known as florfenicol, is a broad-spectrum antibiotic for animals, mainly used for bacterial diseases in cattle, pigs, chickens, ducks, fish and other animals. The structure of florfenicol is similar to that of thiamphenicol, but its antibacterial activity is 10 times that of thiamphenicol; and it is obviously superior to thiamphenicol in terms of antibacterial broad-spectrum and adverse reactions. At present, Florfenicol has become the main antibacterial drug for animals. In view of its excellent efficacy, its application prospect is very broad. Therefore, the synthesis of Florfenicol has been paid great attention. [0003] The structural formula of Florfenicol is as follows: [0004] [0005] The current industrial preparation of Florfenicol mainly takes p-thympheny...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C315/04C07C315/06C07C317/32C07D263/14C07D263/10C07C209/60C07C211/15
CPCC07C209/60C07C315/04C07C315/06C07D263/10C07D263/14C07C317/32C07C211/15
Inventor 王峥徐金雷麻红利余喜明陶保林井庆阳
Owner HUBEI ZHONGMU ANDA PHARMACEUTICAL CO LTD
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