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Method for synthesizing phenylserine derivative based on fixed bed reactor

A fixed-bed reactor, a technology of phenylserine, which is applied in the field of synthesis of phenylserine derivatives, can solve the problems of high pollution, low economy, non-compliance with environmental protection policies, etc., and achieves reduction of environmental pollution, labor and time, and reduction of The effect of emissions

Active Publication Date: 2019-10-15
王喆明 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The synthesis method must use copper sulfate, and in the post-treatment, highly toxic and smelly hydrogen sulfide is used to precipitate copper ions, resulting in a large amount of copper sulfide solid waste, which is a backward process with high pollution and low economy, and does not meet the requirements of The current environmental protection policy requires urgent improvement

Method used

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  • Method for synthesizing phenylserine derivative based on fixed bed reactor

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] like figure 1 Shown is a fixed bed reaction device for synthesizing phenylserine derivatives, including a premixer 1, the premixer 1 is connected with the fixed bed 2, and the connected pipeline is equipped with a liquid pump 11 and a control valve 12; the lower outlet of the fixed bed 1 ( or called the outlet) is connected to the inlet of the first separator 3, and the connected pipeline is equipped with a liquid pump 11 and a control valve 12; the outlet of the first separator 3 is connected to the inlet of the second separator 4, and the connected pipeline is equipped with Liquid pump 11 and control valve 12, water storage tank 10 and the inlet of the second separator 4 are connected, and the connected pipeline is equipped with liquid pump 11, control valve 12 and flow meter 13 (or called flow controller); the second separator 4 They are respectively connected to the first storage tank 5, the second storage tank 6, and the third storage tank 7, and each connecting pi...

Embodiment 2

[0037] Adopt the synthetic method of the p-thiamphenicol phenylserine of the fixed-bed reactor of embodiment 1, flow process is as follows:

[0038] Each reactor is filled with catalyst and filler in advance. The fixed bed catalyst is copper ion fixed on the chelating resin through complexation. The resin is LSC-910 chelating resin from Lanxiao, and the copper ion loading is 1.5 %; The metal ion adsorption resin is Samyang CLR-08 chelating resin; the adsorption separation resin is Purite C115E resin, and purified water is used to pass through the equipment, the equipment and fillers are thoroughly cleaned, and the washing water is detected by HPLC (230nm absorption wavelength, isocratic elution) to no obvious impurities (50 times the volume of washing water to dissolve the standard, wherein the maximum impurity introduced in the washing water is <0.1%);

[0039] Start the premixer, add raw materials (ie: 4-thiamphenicol benzaldehyde, glycine, phosphate buffered saline, water),...

Embodiment 3

[0043] Adopt the synthetic method of the p-thiamphenicol phenylserine of the fixed-bed reactor of embodiment 1, flow process is as follows:

[0044] Each reactor is filled with catalyst and filler in advance. The fixed bed catalyst is copper ion fixed on the chelating resin through complexation. The resin is LSC-910 chelating resin from Lanxiao, and the copper ion loading is 1.5 %, the metal ion adsorption resin is LSC-910 chelating resin from Lanxiao, the adsorption separation resin is Purite C115E resin, and purified water is used to pass through the equipment, the equipment and packing are thoroughly cleaned, and the washing water is detected by HPLC (230nm absorption wavelength, isocratic elution) to no obvious impurities (50 times the volume of washing water to dissolve the standard, wherein the maximum impurity introduced in the washing water is <0.1%);

[0045] Start the premixer, add the materials p-thymphenylbenzaldehyde, glycine, phosphate buffer salt, and purified w...

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Abstract

The invention provides a method for synthesizing a phenylserine derivative based on a fixed bed reactor. The method comprises the following steps: raw materials are uniformly mixed in a premixer, andare maintained at a certain temperature, then the obtained mixture enters a fixed bed from the upper part, and contacts with a contact to undergo an Adol reaction, and the above produced enters a first separator from the outlet of the fixed bed to remove a small amount of metal ions, and then flows through a second separator to separate the product and byproducts in order to obtain the high-purityphenylserine derivative product. Solvent materials used and involved in the reaction can be recycled after being separated and concentrated. The method has the following advantages: (1) the reactionprocess is simple to operate, and the whole process is a full-flow reaction, so high efficiency and short time are achieved; (2) the solvent and excess raw materials can be recycled, and three wastesare rarely discharged, so the method is green, economical and environmentally friendly; and (3) the method has a low energy consumption and a high yield per unit, so the method suitable for amplifiedproduction.

Description

【Technical field】 [0001] The invention relates to the field of chemical industry, in particular to a method for synthesizing phenylserine derivatives based on a fixed-bed reactor. 【Background technique】 [0002] Phenylserine derivatives are important pharmaceutical intermediates and chemical intermediates, especially 4-thiamphenicyl phenylserine, 4-nitrophenylserine, etc., which are widely used in the preparation of human antibiotics and poultry and livestock antibiotics. Drugs such as chloramphenicol, thiamphenicol, florfenicol and so on. [0003] The industrial production method of phenylserine derivatives is mainly the traditional chemical synthesis method, using mono / multi-substituted benzaldehyde, glycine, copper sulfate, and ammonia water as raw materials, heating and stirring at 45-50°C for 30 hours to obtain mono / multi-substituted copper phenylserine salt, then add water to dissolve the copper salt, and then pass through hydrogen sulfide gas to remove copper ions, f...

Claims

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Application Information

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IPC IPC(8): C07B37/00C07B63/00C07C227/16C07C227/40C07C229/36C07C315/04C07C315/06C07C317/48B01J8/02B01J8/04
CPCC07B37/00C07B63/00C07C227/16C07C227/40C07C315/04C07C315/06B01J8/0242B01J8/0449C07C229/36C07C317/48
Inventor 王喆明谭昊
Owner 王喆明
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