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Method for recovering copper salt and ethanol from D,L-threo-p-methylsulfonylphenyl serine ethyl ester stock solution

A technology of thiamphenyl phenylserine ethyl ester mother liquor and thiamphenyl phenylserine ethyl ester, which is applied in the fields of medicine and chemical industry, can solve problems such as decline, and achieve the effects of reducing COD, reducing wastewater treatment costs, and reducing product costs

Inactive Publication Date: 2018-11-30
江苏八巨药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The technical problem to be solved in the present invention is to provide a kind of friendly environment and economic Advanced recycling process greatly reduces COD in wastewater, greatly reduces the cost of wastewater treatment, and reduces product costs

Method used

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  • Method for recovering copper salt and ethanol from D,L-threo-p-methylsulfonylphenyl serine ethyl ester stock solution
  • Method for recovering copper salt and ethanol from D,L-threo-p-methylsulfonylphenyl serine ethyl ester stock solution
  • Method for recovering copper salt and ethanol from D,L-threo-p-methylsulfonylphenyl serine ethyl ester stock solution

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Add 300g of the esterification reaction mother liquor and 600g of the free D,L-threo-p-thymphenylphenylserine ethyl ester mother liquor into a 1000ml three-necked flask. After stirring, turn on the heating to 70°C for distillation, distill to 105°C, and ethanol Distillation column rectification; continue to add 5g of activated carbon to the mother liquor at 105°C, keep it for 2 hours for hydrolysis and decolorization, cool down to 30°C, filter, add 16g of copper sulfate pentahydrate to the filtrate, add liquid alkali dropwise to adjust PH=5, stir for 1 hour, Filter and dry. The results are shown in Table 1

Embodiment 2

[0033] Add 300g of the esterification reaction mother liquor and 1200g of the free D,L-threo-p-thymphenylphenylserine ethyl ester mother liquor to a 2000ml three-necked flask. After stirring, turn on the heating to 70°C for distillation, and then distill to 105°C. Rectification in the distillation column; continue to add 7.5g of activated carbon to the mother liquor at 110°C, keep it for 2 hours for hydrolysis and decolorization, cool down to 30°C, filter, add 16g of copper sulfate pentahydrate to the filtrate, add liquid alkali dropwise to adjust the pH to 5, and stir for 1 hour , filtered and dried. The results are shown in Table 1

Embodiment 3

[0035] Add 300g of esterification reaction mother liquor and 900g of free D,L-threo-p-thymphenylphenylserine ethyl ester mother liquor to a 2000ml three-neck flask, after stirring, turn on the heating to 70°C for distillation, then distill to 105°C, and ethanol Distillation column rectification; continue to add 6g of activated carbon to the mother liquor at 110°C, keep it for 2 hours for hydrolysis and decolorization, cool down to 30°C, filter, add 16g of copper sulfate pentahydrate to the filtrate, add liquid alkali dropwise to adjust PH=6.5, stir for 1 hour, Filter and dry. The results are shown in Table 1

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Abstract

In view of defects of the existing treatment technologies for reacted stock solutions of DL-threo-p-methylsulfonylphenyl serine ethyl ester, the invention provides a route for synthesizing D-threo-p-methylsulfonylphenyl serine ethyl ester from p-methylsulfonylphenyl serine copper. The route comprises the steps of carrying out an esterification reaction, subjecting filter liquor, i.e., an esterification reaction stock solution, produced during the obtaining of D,L-threo-p-methylsulfonylphenyl serine ethyl ester sulfate, to suction filtering, subjecting a free D,L-threo-p-methylsulfonylphenyl serine ethyl ester stock solution, produced during the obtaining of a D,L-threo-p-methylsulfonylphenyl serine ethyl ester, to suction filtering, carrying out mixing, distilling, hydrolyzing, pH adjusting, copper salt preparing, and recovering ethanol and a copper salt (i.e., p-methylsulfonylphenyl serine copper). The ethanol and the p-methylsulfonylphenyl serine copper recovered can be applicable tonext-step production. The content of CODs in wastewater is greatly lowered, the cost of wastewater treatment is greatly reduced, and the product cost is reduced. The invention has an important significance in reducing raw material cost, reducing wastewater treatment cost and promoting the sustainable development of enterprises.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, and relates to a series of novel preparation methods of broad-spectrum antibacterial drug intermediates of chloramphenicol special for veterinary medicine. More specifically, it relates to a method for recovering copper salt and ethanol from D,L-threo-p-thymphenylphenylserine ethyl ester mother liquor. Background technique [0002] Chemical name: 4-Methylsulfone Phenylserine Copper, the English name is 4-Methylsulfone Phenylserine Copper, and the structural formula is as follows. [0003] [0004] The following is a relatively mature synthesis process of copper p-thymphenylphenylserine: [0005] Using p-thiamphenicol benzaldehyde, glycine and copper sulfate as reaction raw materials, water as reaction solvent, and adding liquid caustic soda dropwise to synthesize copper p-thiamphenicol phenylserine. [0006] Florfenicol (Florfenicol) is a new veterinary-specific broad-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C315/04C07C317/48C07C29/80C07C31/08
CPCC07C29/80C07C315/04C07C317/48C07C31/08
Inventor 楚玮明孔立程焕达王小明程加铭陈恬
Owner 江苏八巨药业有限公司
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