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Synthesis process for DL-p-methyl sulfone benzene ethyl serinate water-carrying esterification

A technology of methylsulfonylphenylserine ethyl ester and water ester, which is applied in the synthesis field of amino acid esterification, can solve the problems of unfavorable solvent recovery and mechanical application, and achieve the effects of improving equipment utilization, simple solvent recovery method and high purity

Active Publication Date: 2018-05-15
SHANDONG HANXING PHARM TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The esterification reaction effectively improves the reaction yield by using an additional water-carrying agent, but due to the need to use a variety of solvents, it is unfavorable for the recovery and application of solvents in industry

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 350g copper salt (outside standard mass content 82%) in 1000ml there-necked flask, 875g ethanol, drip 207g (0.59 times, 3.5 times the amount of copper salt of mole) 98% sulfuric acid under water-bath control condition, dropwise after finishing React at 82-84°C for 3 hours, cool down to 60-65°C and filter while hot, wash the filter cake with 100ml of absolute ethanol, heat up and concentrate the filtrate to evaporate about 85% of the feed ethanol, and apply the evaporated ethanol to the next batch or It is used intensively after treatment (it can also be mixed with new absolute ethanol), until the temperature reaches 92-94°C, add 1050g (3 times) of ethanol with water dropwise, and maintain the temperature during the process of carrying water at 92-94°C. 95% of the ethanol with water is considered as the end of the water) After the water is over, the temperature is controlled at 0-25°C, and the feed liquid is slowly poured into ice water, and after mixing evenly, add a...

Embodiment 2

[0033] Add 350g copper salt (external standard mass content 82%), 875g ethanol in the 1000ml there-necked bottle, add dropwise 224.7g (0.64 times, 3.8 times the copper salt amount of mole) 98% sulfuric acid under water bath control condition, after dropwise addition finishes React at 82-84°C for 3 hours, cool down to 60-65°C and filter while it is hot, wash the filter cake with 100ml of absolute ethanol, heat up the filtrate and concentrate to evaporate about 85% of the feed ethanol until the temperature reaches 92-94°C, drop Add 1050g of water-carrying ethanol (3 times), and the temperature of the water-carrying process is maintained at 92-94°C. When (approximately 95% of the water-carrying ethanol is evaporated is regarded as the end of water-carrying), the temperature is controlled at 0-25°C , slowly pour the feed liquid into ice water, mix well, add activated carbon and slowly add 20% sodium sulfide aqueous solution to the feed liquid, stir for 0.2 hours, filter, wash the f...

Embodiment 3

[0035]Add 350g copper salt (external standard mass content 82%), 875g ethanol in the 1000ml there-necked bottle, add dropwise 224.7g (0.64 times, 3.8 times the copper salt amount of mole) 98% sulfuric acid under water bath control condition, after dropwise addition finishes React at 82-84°C for 3 hours, cool down to 60-65°C and filter while it is hot, wash the filter cake with 100ml of absolute ethanol, heat up the filtrate and concentrate to evaporate about 85% of the feed ethanol until the temperature reaches 92-94°C, drop Add 1400g of water-carrying ethanol (4 times), and the temperature of the water-carrying process is maintained at 92-94°C. When (approximately 95% of the water-carrying ethanol is evaporated is regarded as the end of water-carrying), the temperature is controlled at 0-25°C , slowly pour the feed liquid into ice water, mix well, add activated carbon and slowly add 20% sodium sulfide aqueous solution to the feed liquid, stir for 0.2 hours, filter, wash the fi...

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Abstract

The invention discloses a synthesis process for DL-p-methyl sulfone benzene ethyl serinate water-carrying esterification. The synthesis process comprises the following steps: (1) putting a copper saltand absolute ethyl alcohol into a reactor, dropping sulfuric acid to carry out an esterification reaction, and after the reaction is completed, filtering so as to obtain esterification filtrate; (2)heating the esterification filtrate obtained in the step (1), concentrating, performing water-carrying esterification with the absolute ethyl alcohol, and after the water-carrying esterification is completed, performing aftertreatment, thereby obtaining DL-p-methyl sulfone benzene ethyl serinate. The synthesis process is simple in reaction route, high in product yield, good in synthesis product stability and high in purity, and can be adopted to synthesize a key intermediate of a veterinary drug florfenicol and an antibacterial raw material medicine thiamphenicol.

Description

technical field [0001] The invention relates to a synthesis method of amino acid esterification, in particular to a synthesis method of DL-p-thymphenylphenylserine ethyl ester with water. Background technique [0002] In recent years, the application of amino acid esters has become more and more extensive, especially in the chemical industry, pharmaceutical industry, food processing, daily cosmetics and spices industry, agricultural product care and other industries. The application prospect is very broad. [0003] DL-p-thiamphenicol phenylserine ethyl ester, white powdery crystal, is an important pharmaceutical intermediate, such as the key intermediate for the synthesis of veterinary drug florfenicol and antibacterial raw material drug thiamphenicol. Its molecular structure contains amino groups, which is easy to polymerize and oxidize, and has poor stability and is not easy to store for a long time. Although DL-p-thymphenylphenylserine ethyl ester has strong water absorp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C315/04C07C317/48
CPCC07C315/04C07C317/48
Inventor 雷江申屠有德徐健王平牛明举季可洁刘杰
Owner SHANDONG HANXING PHARM TECH CO LTD
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