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Method for preparing Imipenem monohydrate crystals

A technology of monohydrate and imipenem, applied in the direction of organic chemistry, etc., to achieve the effect of low solvent residue, simple and easy process, and less loss of raw materials

Active Publication Date: 2012-06-13
SHENZHEN HAIBIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] None of the above reported preparation methods for the crystallization of imipenem monohydrate involves the problem of reducing solvent residues, and the control of solvent residues is an indicator that must be paid attention to

Method used

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  • Method for preparing Imipenem monohydrate crystals

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Under nitrogen atmosphere, distilled water (200ml) was heated to 40°C. Add the crude imipenem (5.0 g, content about 92%) into distilled water, stir at 40-45°C for 2 minutes, add 1 g of activated carbon, then rapidly cool to 5°C-10°C, filter to remove the activated carbon, and the filtrate Cool down to 10°C, add a small amount of seed crystals, stir for 4 hours at a relatively fast speed, keep the temperature at 2-5°C, filter to obtain 2.5g of imipenem monohydrate crystals, the external standard content is 98.2%, and various organic solvents remain Less than 0.5‰.

[0028] Add 200ml of acetone to the mother liquor, keep stirring at 2-5°C for 1 hour, then start to add 100ml of acetone dropwise, finish dropping in 30 minutes, keep stirring at this temperature for 2 hours, then filter, and recover 1.5g of imipenem monohydrate.

Embodiment 2

[0030] Under nitrogen atmosphere, distilled water (250ml) was heated to 30°C. Add the crude imipenem (5.0 g, content about 92%) into distilled water, stir at 30°C for 2 minutes, add 1 g of activated carbon, then rapidly cool to 5°C-10°C, remove the activated carbon by filtration, and cool the filtrate to Stir rapidly at 5°C for 4 hours, keep the temperature at 2-5°C, and filter to obtain 2.1 g of imipenem monohydrate crystals, with an external standard content of 98.5%, and residual organic solvents of less than 0.5‰.

[0031] Add 250ml of acetone to the mother liquor, keep stirring at 2-5°C for 1 hour, then start to add 100ml of acetone dropwise, finish dropping in 30 minutes, keep stirring at this temperature for 3 hours, then filter, and recover 1.8g of imipenem monohydrate.

Embodiment 3

[0033] Under nitrogen atmosphere, distilled water (150 ml) was heated to 70°C. Add the crude imipenem (5.0 g, content about 92%) into distilled water, stir at 50°C for 2 minutes, add 1 g of activated carbon, then rapidly cool to 5°C-10°C, remove the activated carbon by filtration, and cool the filtrate to 10°C, add a small amount of seed crystals, stir rapidly for 4 hours, keep the temperature at 2-5°C, filter to obtain 2.0g of imipenem monohydrate crystals, the external standard content is 98%, and the residual organic solvents are less than 0.5‰ .

[0034] Add 200ml of acetone to the mother liquor, keep stirring at 10°C for 1 hour, start to add 100ml of acetone dropwise, and finish dropping in 30 minutes, keep stirring at this temperature for 2 hours, then filter, and recover 1.2g of imipenem monohydrate.

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Abstract

The invention discloses a method for preparing Imipenem monohydrate crystals, comprising the following steps: dissolving an Imipenem crude product in water at the temperature of 30-65 DEG C to obtain a solution I; processing the solution I by activated carbon, filtering at the temperature of 5-30 DEG C to obtain a filtrate II; subjecting the filtrate II to precipitation at the temperature of 0-10DEG C, filtering to obtain a filtrate III and purified Imipenem monohydrate crystals; and further adding an organic solvent in the filtrate III, and recovering to obtain an Imipenem monohydrate crudeproduct. The method is simple and feasible, and the obtained Imipenem monohydrate crystals have extra low solvent residue, meets the method requirements on preparing the Imipenem and is suitable for industrialized production.

Description

technical field [0001] The invention relates to a method for preparing a compound, in particular to a method for refining imipenem monohydrate crystals with ultra-low solvent residue. Background technique [0002] Imipenem (imipenem) is a carbapenem extended-spectrum β-lactam antibiotic developed by Merck, which is a compound preparation (trade name: Taineng) is the first marketed carbapenem β-lactam antibiotic. [0003] Imipenem monohydrate crystal (formula I) is a relatively stable form of imipenem, and its purification method has been reported. [0004] [0005] U.S. patents such as US4194047, US4260543, and US4292436 all purify imipenem crude product or a solution containing imipenem by column chromatography and freeze-dry to obtain amorphous imipenem, or subsequently crystallize to obtain imipenem. Ampenem monohydrate. Later, Crocker and Connolly etc. also reported the method (J.Pharm.Sci., 1995,84,226; J.Pharm.Sci., 1995,84,226; J. Pharm. Sci., 1996, 85, 174). ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D477/20C07D477/06
Inventor 朱喜宗任鹏汪小华
Owner SHENZHEN HAIBIN PHARMA
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