Crystal form B of oxazolidone antibacterial drugs as well as preparation method and application of crystal form B
A technology for oxazolidinone and antibacterial drugs, which is applied to the crystal form B of oxazolidinone antibacterial drugs and the field of preparation thereof, can solve the problems of high residual organic solvent, difficult drying, poor stability and the like, and achieves the residual amount of solvent Small, reproducible results
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Embodiment 1
[0025] The preparation of the amorphous solid of embodiment 1 oxazolidinone antibacterial drug free acid
[0026]
[0027] 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%.
[0028] The reaction process is as follows:
[0029]
[0030] 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
[0031] The preparation of the crystal form B of oxazolidinone antibiotics shown in embodiment 2 formula (2)
[0032] 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 acetone (27ml), statically crystallized, filtered with suction, and dried in vacuo. The resulting solid was subjected to powder X-ray diffraction.
Embodiment 3
[0033] The preparation of the crystal form B of oxazolidinone antibiotics shown in embodiment 3 formula (2)
[0034] 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 methyl isobutyl ketone (18ml), statically crystallized, filtered with suction, and dried in vacuo. The resulting solid was subjected to powder X-ray diffraction.
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