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High-purity D-dihydrophenylglycine methyl ester and preparation method thereof

A technology of dihydrophenylglycine methyl ester and dihydrophenylglycine, which is applied in the fields of high-purity D-dihydrophenylglycine methyl ester and preparation thereof, D-dihydrophenylglycine methyl ester and preparation thereof, and can Solve problems such as high cost, complex process and harsh conditions

Pending Publication Date: 2021-09-14
NORTH CHINA PHARMA COMPANY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of this, the present invention provides a method for preparing high-purity D-dihydrophenylglycine methyl ester to solve the problems of high cost, complicated process and harsh conditions in the preparation method of D-dihydrophenylglycine methyl ester in the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a 50L reaction tank, add 20L of methanol, add 5Kg of D-dihydrophenylglycine under stirring, after stirring evenly, reflux at 60-65°C for 0.5h, cool down at 45-55°C, keep a slight positive pressure of 0.005MPa, and add concentrated sulfuric acid 5Kg, temperature control below 50°C, after the dropwise addition, maintain the temperature in the reactor at 59°C, reflux for 3.5h, and the reaction ends. Then carry out vacuum distillation, and the vacuum degree in the reactor is maintained at 0.03MPa. After the mass content of methanol in the solution in the reaction tank reaches 10%, the vacuum distillation is stopped. Add methanol 20L, reflux for 4h, and the reaction ends. Then carry out vacuum distillation, and the vacuum degree in the reactor is maintained at 0.03MPa. After the mass content of methanol in the solution in the reaction tank reaches 10%, the vacuum distillation is stopped. This is repeated three times to reach 0.3% of D-dihydrophenylglycine.

Embodiment 2

[0025] In a 50L reaction tank, add 20L of methanol, add 5Kg of D-dihydrophenylglycine under stirring, after stirring evenly, reflux at 60-65°C for 1.0h, cool down at 45-55°C, maintain a slight positive pressure of 0.007MPa, and add concentrated sulfuric acid 5Kg, temperature control below 50°C, after dropwise addition, keep the temperature inside the reactor at 60°C, reflux for 5h, and the reaction ends. Then carry out vacuum distillation, and the vacuum degree in the reactor is maintained at 0.03MPa. After the mass content of methanol in the solution in the reaction tank reaches 10%, the vacuum distillation is stopped. Add methanol 20L, reflux for 4.5h, and the reaction ends. Then carry out vacuum distillation, and the vacuum degree in the reactor is maintained at 0.03MPa. After the mass content of methanol in the solution in the reaction tank reaches 10%, the vacuum distillation is stopped. This is repeated three times to reach 0.3% of D-dihydrophenylglycine.

Embodiment 3

[0027] In a 50L reaction tank, add 20L of methanol, add 5Kg of D-phenylglycine while stirring, after stirring evenly, reflux at 60-65°C for 0.5h, cool down to -10-0°C, maintain negative pressure, and add 5Kg of thionyl chloride at one time After the addition, the temperature in the reactor was maintained at 59° C., and the reaction was completed by refluxing for 3.5 hours. Then carry out vacuum distillation, and the vacuum degree in the reactor is maintained at 0.03MPa. After the mass content of methanol in the solution in the reaction tank reaches 15%, stop vacuum distillation, cool down and crystallize, drop to 0°C, stir for 30-60min, then centrifuge, and vacuum dry at 50°C for 8h to obtain D-phenylglycine methyl ester salt Salt 4.80Kg.

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Abstract

The invention discloses high-purity D-dihydrophenylglycine methyl ester and a preparation method thereof, and belongs to the field of pharmaceutical chemicals, and the preparation method comprises the following steps: uniformly mixing and stirring D-dihydrophenylglycine and methanol, carrying out heating reflux, adding a reaction reagent concentrated sulfuric acid or thionyl chloride, and carrying out reflux reaction to obtain the high-purity D-dihydrophenylglycine methyl ester. According to the preparation method, the existing preparation process is changed, the content of phenylglycine methyl ester in the product is less than 0.67%, and due to the innovative preparation mode, the product cost is reduced. In addition, the production process is simple and easy to operate, low in production cost and beneficial to industrial production.

Description

technical field [0001] The invention relates to a D-dihydrophenylglycine methyl ester and a preparation method thereof, in particular to a high-purity D-dihydrophenylglycine methyl ester and a preparation method thereof, belonging to the field of medicine and chemical industry. Background technique [0002] D-dihydrophenylglycine methyl ester is the side chain of enzymatic ampicillin. [0003] Sinochem DSM Pharmaceutical Co., Ltd. Dutch company "Method for producing cephradine", application number 201080057051.8. Propose to use inert gas protection such as nitrogen in the production process, the phenylglycine methyl ester 0.87% in the D-dihydrophenylglycine methyl ester that can be produced, to prepare high-quality cephradine. [0004] The main problem of the above method is: to degas methanol with nitrogen, the oxygen content needs to be lower than 100ppm, the cost is high, and it seriously affects the preparation of enzymatic antibiotics. Contents of the invention [0...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/18C07C227/40C07C229/32
CPCC07C227/40C07C227/18C07C2601/16C07B2200/07C07C229/32
Inventor 张军立段志钢王新辉薛同山刘倩张致一赵庆年李珠张冲翟梦刘磊师书迪白米册徐颖
Owner NORTH CHINA PHARMA COMPANY
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