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D-phenylglycine methyl ester phosphate crystal, preparation method and solution

A technology of phenylglycine methyl ester and phenylglycine, which is applied in the field of D-phenylglycine methyl ester phosphate crystallization and preparation method, and solution field, can solve the problems of equipment corrosion, low synthesis conversion rate, etc., and achieves the benefit of production amplification and improved reaction effect. , the effect of significant economic benefits

Pending Publication Date: 2020-11-10
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a crystallization of D-phenylglycine methyl ester phosphate and its preparation method and solution to solve the problems of low conversion rate of subsequent enzymatic synthesis and serious corrosion of equipment in the related art

Method used

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  • D-phenylglycine methyl ester phosphate crystal, preparation method and solution
  • D-phenylglycine methyl ester phosphate crystal, preparation method and solution
  • D-phenylglycine methyl ester phosphate crystal, preparation method and solution

Examples

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Embodiment 1

[0042] The preparation of embodiment 1D-phenylglycine methyl ester phosphate crystal

[0043]In a 200L reaction tank, add 80L of methanol, add 20Kg of D-phenylglycine while stirring, after stirring evenly, add 20Kg of phosphoric acid, and control the temperature below 40°C. After the feeding was completed, the temperature in the reaction tank was maintained at 75° C., and the reflux reaction was carried out for 2 hours, and the reflux reaction was completed. Then carry out vacuum dehydration, adopt the mode of vacuum distillation, specifically, the vacuum degree in the reaction tank is maintained at 0.04~0.06MPa, after the mass content of methanol in the solution in the reaction tank reaches 2%, stop the vacuum distillation. Then add methanol 60L, continue the reflux reaction for 1h, after the reflux reaction ends, distill under reduced pressure, and cool down to crystallize after the mass content of methanol in the solution in the reaction tank reaches 2%, repeat this 5 times...

Embodiment 2

[0049] The preparation of embodiment 2 cephalexin

[0050] Suspend 20 g of 7-aminodeacetoxycephalosporanic acid (7-ADCA) in 100 mL of water, and control the temperature at 25°C. The mixture was stirred for 5 minutes while maintaining the pH at 7.0 by adding 15% aqueous ammonia solution, and 10 g of immobilized enzyme was added. Next, 25 g of D-phenylglycine methyl ester phosphate crystals were added at a constant rate within 90 min. Once all the D-phenylglycine methyl ester phosphate crystallization was added, the pH was maintained at 7.0 by adding 15% aqueous ammonia or by adding 30% aqueous sulfuric acid. After 230 min, the pH was adjusted by adding 30% aqueous sulfuric acid to 5.8. During the reaction, samples were taken and analyzed by high performance liquid chromatography (High Performance Liquid Chromatography, HPLC). The analysis results are shown in Table 2.

[0051] Table 2 Sampling analysis results for the preparation of cephalexin based on D-phenylglycine methyl...

Embodiment 3

[0064] The preparation of embodiment 3 ampicillin

[0065] Suspend 20 g of 6-aminopenicillanic acid (6-APA) in 100 mL of water, and control the temperature at 25°C. The mixture was stirred for 5 minutes while maintaining the pH at 7.0 by adding 15% aqueous ammonia solution, and 10 g of immobilized enzyme was added. Next, 25 g of D-phenylglycine methyl ester phosphate crystals were added at a constant rate within 90 min. Once all of the D-phenylglycine methyl ester phosphate crystallization was added, the pH was maintained at 7.0 by the addition of 15% aqueous ammonia or by the addition of 30% aqueous sulfuric acid. After 230 minutes, the pH was adjusted to 5.8 by the addition of 30% aqueous sulfuric acid . During the reaction, samples were taken and analyzed by HPLC, and the analysis results are shown in Table 5.

[0066] Table 5 Sampling analysis results for the preparation of ampicillin based on the crystallization of D-phenylglycine methyl ester phosphate

[0067]

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Abstract

The invention discloses a D-phenylglycine methyl ester phosphate crystal, a preparation method and a solution, and the preparation method comprises the following steps: step a, adding Dphenylglycine and methanol into a reaction tank, uniformly stirring, and feeding phosphoric acid; step b, after the phosphoric acid is fed, carrying out reflux reaction; c, after the reflux reaction in the step b isfinished, carrying out vacuum dehydration, and then repeating the following operations for n times: adding methanol, continuously carrying out the reflux reaction, and carrying out vacuum dehydrationafter the reflux reaction is finished; and d, adjusting the pH value to be acidic, adding the Dphenylglycine methyl ester phosphate seed crystal for crystallization, and drying to obtain the Dphenylglycine methyl ester phosphate crystal. The problems of low subsequent enzymatic synthesis conversion rate and severe corrosion to equipment in the related art are solved.

Description

technical field [0001] The invention relates to the technical field of medicine and chemical industry, in particular to a D-phenylglycine methyl ester phosphate crystallization, a preparation method and a solution. Background technique [0002] At present, the side chains of enzymatic ampicillin, cephalexin, and cefaclor are prepared based on the hydrochloride or hemisulfate of D-phenylglycine methyl ester, for example, the literature "Cefaclor active side chain phenylglycine methyl ester hydrochloride The synthesis method of D-phenylglycine methyl ester hydrochloride mentioned in "Synthesis", another example, the synthesis method of the hemisulfate of D-phenylglycine methyl ester mentioned in the patent document CN107074742A. [0003] The main problem of the above-mentioned method is: whether it is the preparation of hydrochloride or hemisulfate of D-phenylglycine methyl ester, on the one hand, the subsequent enzymatic synthesis conversion rate is on the low side, only 96%,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/36C07C227/18C07C227/42C07D501/22C07D499/68C07D499/06C07D501/59C07D501/04
CPCC07B2200/13C07C229/36C07D499/06C07D499/68C07D501/04C07D501/22C07D501/59
Inventor 龚俊波张军立侯宝红尚泽仁吴送姑王新辉臧飞李小瑞杨婷
Owner TIANJIN UNIV
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