Suspension crystallization method for preparing crystal form I of linezolid

A technology of linezolid and suspension crystallization, which is applied in the field of compound preparation, can solve the problems that the yield of linezolid crystal form I is not higher than 90%, the difficulty of solvent recovery, and the inability to directly reuse, etc., to achieve high product yield , the effect of energy consumption reduction

Active Publication Date: 2012-04-04
ZHEJIANG LEPU PHARMA CO LTD
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  • Abstract
  • Description
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Problems solved by technology

However, the above-mentioned methods for preparing crystalline form I of linezolid (J. Med. Chem. 39(3): 673-679, 1996; CN102070548) all use or produce mixed solvents, which makes solvent recovery difficult and cannot be directly reused. The yield of linezolid crystal form I is not higher than 90%

Method used

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  • Suspension crystallization method for preparing crystal form I of linezolid
  • Suspension crystallization method for preparing crystal form I of linezolid

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Add 100g of linezolid crystal form II to a 1000ml flask, add 100g of water, stir and heat to 105°C to make a suspension, cool down to 100°C for crystallization, filter while hot at 90°C, and vacuum dry the filter cake at 30°C to obtain linezolid Azolamide crystal form I is 95.2g, and the yield is 95.2%. The X-ray powder diffraction (XRPD) pattern of Linezolid Form I is shown in figure 1 .

Embodiment 2

[0021] Add 100g of linezolid mixed crystals (Form I and Form II) into a 1000ml flask, add 300g of water, stir and heat to 100°C to make a suspension, cool to 85°C for crystallization, then cool to 0°C and filter, filter The cake was vacuum-dried at 50°C to obtain 99.1 g of Linezolid Form I, with a yield of 99.1%.

Embodiment 3

[0023] 100 g of linezolid crystalline form II was added to a 1000 ml flask, 290 g of the mother liquor was filtered by adding Example 2, and the rest was the same as in Example 2 to obtain 99.3 g of linezolid crystalline form I with a yield of 99.3%.

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Abstract

The invention discloses a suspension crystallization method for preparing a crystal form I of linezolid. The method comprises the following steps of: mixing 1 to 10 weight part of water and 1 weight part of linezolid, heating to the temperature of between 95 and 105DEG C to obtain suspension, crystallizing at the temperature of between 70 and 100DEG C, filtering at the temperature of between 0 and 90DEG C, and performing vacuum drying on a filter cake at the temperature of between 30 and 90DEG C to obtain the crystal form I of the linezolid. The method has the advantages that: water is taken as a suspension solvent, organic solvents are not used at all, the method is green, safe, environment-friendly and pollution-free, the product yield is high, the filter cake is not required to be washed, the filtered mother solution can be repeatedly used, the volume of the mother solution cannot be increased due to reuse, the energy consumption in the production process is obviously reduced, and clean production can be realized.

Description

technical field [0001] The present invention relates to a preparation method of a compound, in particular to a method for preparing linezolid crystal form I by a suspension crystallization method. Background technique [0002] Linezolid, chemical name: (S)-N-[[3-(3-fluoro-4-morpholinyl)phenyl]-2-oxo-5-oxazolidinyl]methylacetamide. It is an antibacterial drug used to treat infections caused by various bacteria. Molecular formula is C 16 h 20 FN 3 o 4 , the structural formula is as follows: [0003] [0004] US Patent US5688792, European Patent EP717738, Israeli Patent IL110802, Canadian Patent CA2168560, International Patent WO95 / 07171 and Chinese Patents CN101128442, CN101220001, CN101774978, J. Med. Chem. 39(3): 673-679, 1996; Tetrahedron Lett ., 40(26): 4855-4856, 1999; China Journal of Pharmaceutical Industry, 41(1): 62-63, 2010, disclosed linezolid and its preparation method. [0005] Linezolid exists in several crystalline forms. J. Med. Chem. 39(3): 673-679,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D263/20
Inventor 洪华斌管宜溪袁慎峰孔佳郎洪林冬
Owner ZHEJIANG LEPU PHARMA CO LTD
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