Preparation method of p-methyl sulfone phenyl ethyl serinate

A technology for methylsulfonyl phenylserine ethyl ester and methylsulfonyl phenylserine ethyl ester, which is applied in the field of preparation of p-methylsulfonyl phenylserine ethyl ester, can solve problems such as failure to meet requirements, cancellation of production qualifications, and the like, and achieve the effect of solving environmental pollution

Inactive Publication Date: 2015-08-26
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since 2008, many chemical production enterprises have been closed for rectification because the treatment of "three wastes" has not met the requirements, and some enterprises with serious pollution have even been disqualified from production

Method used

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  • Preparation method of p-methyl sulfone phenyl ethyl serinate

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Comparison scheme
Effect test

Embodiment 1

[0015] Synthesis of p-Methylsulfonyl Phenylserine

[0016] Dissolve 20g of copper p-methylsulfonylphenylserine in sodium hydroxide solution (6g NaOH dissolved in 84mL water), add Na 2 S solution (12.1g Na 2 S was dissolved in 17 mL of water), stirred mechanically for 4 hours, then added 8 g of activated carbon to the mixture, stirred mechanically for 1 hour, and filtered with suction. The filtrate was transferred to a 250mL three-necked flask, concentrated hydrochloric acid was added dropwise to adjust the pH to 3, the crystals were concentrated, and filtered with suction to obtain 13.39g of p-methylsulfonylphenylserine with a yield of 75.4%.

Embodiment 2

[0018] Synthesis of p-Methylsulfonyl Phenylserine

[0019] Dissolve 20g of copper p-methylsulfonylphenylserine in sodium hydroxide solution (6g NaOH dissolved in 84mL water), add Na 2 S solution (12.1g Na 2 S was dissolved in 17 mL of water), stirred mechanically for 4 hours, then added 8 g of activated carbon to the mixture, stirred mechanically for 1 hour, and filtered with suction. The filtrate was transferred to a 250 mL three-necked flask, concentrated hydrochloric acid was added dropwise to adjust the pH to 4, the crystals were concentrated, and filtered with suction to obtain 13.5 g of p-methylsulfonyl phenylserine with a yield of 76%.

Embodiment 3

[0021] Synthesis of p-Methylsulfonyl Phenylserine

[0022] Dissolve 20g of copper p-methylsulfonylphenylserine in sodium hydroxide solution (6g NaOH dissolved in 84mL water), add Na 2 S solution (12.1g Na 2 S was dissolved in 17 mL of water), stirred mechanically for 4 hours, then added 8 g of activated carbon to the mixture, stirred mechanically for 1 hour, and filtered with suction. The filtrate was transferred to a 250 mL three-necked flask, concentrated hydrochloric acid was added dropwise to adjust the pH to 5, the crystals were concentrated, and filtered with suction to obtain 13.85 g of p-methylsulfonyl phenylserine with a yield of 78%.

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Abstract

The invention discloses a preparation method of p-methyl sulfone phenyl ethyl serinate and belongs to the technical field of a synthetic technology of veterinary drugs and pharmaceutical intermediates. According to the technical scheme, the preparation method is characterized in that p-methyl sulfone phenyl serine copper is dissolved in a sodium hydroxide solution, an Na2S solution is added to precipitate Cu<2+>, activated carbon is added to adsorb excess S<2->, the mixture is mechanically agitated and subjected to suction filtration, hydrochloric acid is added to a filtrate to regulate pH to be 3-7, and the mixture is subjected to condensation crystallization and suction filtration to obtain p-methyl sulfone phenyl serine; the p-methyl sulfone phenyl serine is dissolved in absolute ethyl alcohol, concentrated sulfuric acid is added, the mixture is subjected to reflux for 4 h, cooling crystallization and suction filtration, a filter cake is dissolved in water, a saturated Na2CO3 solution is added to regulate pH to be neutral, and the p-methyl sulfone phenyl ethyl serinate is obtained after suction filtration. The preparation method has the advantages as follows: the Na2S solution is added in an alkaline environment to remove Cu ions, the excess S<2-> is removed through activated carbon adsorption, and production of toxic and irritant gas H2S through combination of S ions and H ions is avoided, so that the problem of environmental pollution is solved effectively.

Description

Technical field [0001] The invention belongs to the technical field of synthesis of veterinary drugs and pharmaceutical intermediates, and specifically relates to a preparation method of ethyl p-methylsulfone phenylserine. Background technique [0002] Ethyl p-methylsulfonyl phenylserine, white crystal, molecular formula: C 12 H 17 NO 5 S, slightly soluble in water, the structure is as follows: [0003] [0004] P-methylsulfonyl phenylserine ethyl ester is a key intermediate for the synthesis of broad-spectrum antibiotics such as thiamphenicol and florfenicol. Thiamphenicol, also known as Thiamphenicol, Thiamphenicol, white crystals, odorless, is a broad-spectrum antibiotic of the same type as chloramphenicol, and is caused by Haemophilus influenzae, Escherichia coli, Salmonella, etc. Respiratory tract, urethra, intestinal infections and other infections have a good therapeutic effect, and have long curative effects and small side effects. Florfenicol, also known as fluprofen and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C317/48C07C315/04
Inventor 李世宁姜玉钦毛龙飞寇丽栋李幸娟田东东贾淑红徐桂清李伟
Owner HENAN NORMAL UNIV
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