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Method for preparing and crystallizing sulbactam pivoxyl

A technology of sulbactam pivoxil and sulbactam acid, which is applied in the field of preparation and crystallization of sulbactam pivoxil, can solve the problems of adding expensive catalysts, poor product quality, long reaction time, etc., and achieve high product yield, Short reaction time and good stability

Active Publication Date: 2013-03-20
JIANGXI FUSHINE PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0034] The technical problem to be solved by the present invention is to provide a new sulbactam pix to overcome the above defects such as long reaction time, cumbersome operation, poor product quality, low yield, need for purification, need to add expensive catalyst and high-risk operation. Ester preparation and crystallization method

Method used

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  • Method for preparing and crystallizing sulbactam pivoxyl
  • Method for preparing and crystallizing sulbactam pivoxyl
  • Method for preparing and crystallizing sulbactam pivoxyl

Examples

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Embodiment 1

[0056] 1) Preparation of sulbactam calcium salt

[0057] Inject 233L of ethanol into a 500L reactor, add 23.3kg of sulbactamic acid, control the temperature at 10-15°C, stir to dissolve, add 6.2kg of potassium hydroxide, control the temperature at 10-15°C, stir for 1.0 hours, then centrifuge and dry 26.3kg of sulbactam potassium salt was dried, with a yield of 97.0% and a purity of 97.0%.

[0058] 2) Preparation of sulbactam pivoxil

[0059] Suspend 26.3kg of sulbactam potassium salt in 123L of DMF, stir evenly, then add 17.6kg of chloromethyl pivalate dropwise, control the temperature at 10-15°C, and after 8.0 hours of reaction, slowly add 185L of water and 148L of isopropanol The mixed solution was stirred for 1.0 hour, and centrifuged and dried to obtain 31.9kg of crystalline sulbactam pivoxil, with a yield of 95% and a purity of 99.3% (see figure 1 , where peak A is sulbactam pivoxil).

Embodiment 2

[0061] 1) Preparation of sulbactam calcium salt

[0062] Inject 300L of ethanol into a 500L reactor, add 23.3kg of sulbactamic acid, control the temperature at 10-15°C, stir to dissolve, add 16.8kg of 25% ammonia water, control the temperature at 10-15°C, stir for 1.5 hours, then centrifuge and dry Dry 24.4kg of sulbactam ammonium salt, yield 97.5%, purity 97.1%.

[0063]2) Preparation of sulbactam pivoxil

[0064] Suspend 24.4kg of sulbactam ammonium salt in DMF123L, stir evenly, then add 18.0kg of chloromethyl pivalate dropwise, control the temperature at 10-15°C, react for 7.0 hours, slowly add 185L of water and 148L of isopropanol The mixed solution was stirred for 1.0 hour, and was centrifuged and dried to obtain crystalline sulbactam pivoxil 32.3kg, yield 95.5%, and purity 99.2%.

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Abstract

The invention provides a method for preparing and crystallizing sulbactam pivoxyl, and the method comprises the following steps of: (1) pumping a solvent into a reaction kettle, adding sulbactam acid into the solvent, controlling the temperature, stirring for dissolving, adding alkali into the mixture, controlling the reaction temperature, stirring for complete reaction, and then carrying out centrifugal drying to obtain sulbactam salt; and (2) suspending the sulbactam salt into the solvent, evenly stirring, dropwise adding chloromethyl pivalate, controlling the reaction temperature, adding a mixed solution of water and organic solvent into the mixture after the reaction is completely carried out, stirring, crystallizing and carrying out centrifugal drying to obtain the sulbactam pivoxyl. The method has the advantages that 1) the product is high in yield; 2) the product is crystalline solid, and is good in stability and high in purity; 3) the reaction time is short; 4) the reaction conditions are mild, and the method does not need catalyst and high-risk hydrogenation reaction; and 5) the product is simple in separation operation, can be directly filtered and separated after reaction, and does not need the steps, such as extracting, distilling, high-risk hydrogenation, refining and passing column, which are complicated in operation, so that the batch production period can be greatly shortened.

Description

technical field [0001] The invention relates to a preparation and crystallization method of sulbactam pivoxil. Background technique [0002] The structural formula of sulbactam pivoxil is [0003] [0004] Sulbactam pivoxil is a β-lactamase inhibitor developed by Pfizer of the United States. Phase III clinical studies have been conducted in the United States and Japan. It can be used to treat respiratory tract infections, genitourinary system infections, skin And soft tissue infection, oral infection, such as meningitis, bacterial endocarditis, peritonitis, osteomyelitis, typhoid and paratyphoid and other infectious diseases. As a β-lactamase inhibitor that can be taken orally directly, sulbactam pivoxil can be absorbed in the gastrointestinal tract, which overcomes the shortcomings of poor oral absorption and low blood concentration of sulbactam, and is mainly used for the production of amoxicillin Compound preparation of sulbactam pivoxil. With the implementation of ...

Claims

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Application Information

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IPC IPC(8): C07D499/86C07D499/08
Inventor 柴建华刘亚林许蓓珍
Owner JIANGXI FUSHINE PHARMA CO LTD
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