Crystal form C of oxazolidone antibacterial drug and preparation method and application of crystal form C
A technology for oxazolidinone and antibacterial drugs, which is applied to the crystal form C of oxazolidinone antibacterial drugs and its preparation field, which can solve the problems of high organic solvent residue, difficulty in drying, poor stability, etc., and achieve reproducibility Good, the effect of small amount of solvent residue
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Embodiment 1
[0026] Example 1 Preparation of the Amorphous Solid of the Free Acid of Oxazolidinone Antibacterial Drugs
[0027]
[0028] According to European patent EP2940024A1, the compound of formula (3) is synthesized, the compound of formula (3) (197.3g, 0.3mol) is dissolved in the mixed solvent of methanol (2.5L) and tetrahydrofuran (2.5L), and the high-purity nitrogen is replaced. 10% Pd / C (40 g) was added to replace the hydrogen, and the hydrogenation reaction was carried out at normal temperature and pressure overnight. TLC (dichloromethane / methanol=20:1) detected that the reaction was complete. After suction filtration, the filter cake was washed with N,N-dimethylformamide, and the filtrate was spin-dried to obtain 118.7 g of light yellow solid with a yield of 83%.
[0029] The reaction process is as follows:
[0030]
[0031] Detection by liquid phase: the enantiomeric purity is 99.1% and the sum of impurities including 6 diastereoisomers is 0.9%. The resulting solid was...
Embodiment 2
[0032] The preparation of the crystal form C of the oxazolidinone antibacterial drug shown in embodiment 2 formula (2)
[0033] Get the amorphous oxazolidinone antimicrobial drug free acid (3 g) prepared in Example 1 and mix it with dimethyl sulfoxide (9 ml), stir and dissolve to obtain a clear solution. The clear solution was mixed with methyl tert-butyl ether (27ml), statically crystallized, filtered with suction, and dried in vacuo. The resulting solid was subjected to powder X-ray diffraction.
Embodiment 3
[0034] Example 3 Preparation of Form C of Oxazolidinone Antibacterial Drugs Shown in Formula (2)
[0035] Take the amorphous oxazolidinone antimicrobial drug free acid (3 g) prepared in Example 1 and mix it with N,N-dimethylformamide (9 ml), stir and dissolve to obtain a clear solution. The clear solution was mixed with tetrahydrofuran (36ml), statically crystallized, filtered with suction, and dried in vacuo. The resulting solid was subjected to powder X-ray diffraction.
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