Preparation method of linezolid crystal form
A technology of linezolid and crystal form, applied in the field of preparation of linezolid crystal form, can solve the problems of harsh reaction conditions such as temperature, difficult industrial application, complicated reaction process, etc. good repeatability
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Embodiment 1
[0019] Example 1 Preparation of crystalline form III of linezolid using ethyl acetate / n-heptane
[0020] Compound 1 (500 g, 1.48 mol) was added into ethyl acetate (15 L), heated to dissolve, and then the solution was poured into n-heptane (15 L) to cool and stir for 1 h to crystallize. After filtration, the resulting solid was dried under reduced pressure at 50°C to constant weight. The target product (468 g, off-white solid) was obtained with a yield of 93.6%, HPLC: 99.8%. After testing, its XRPD pattern is as follows figure 1 shown.
Embodiment 2
[0021] Example 2 Screening test for preparation conditions of linezolid crystal form III
[0022] The inventor further carried out a condition screening test for the optimal preparation conditions of the crystal form III. Except for the difference in the types of solvents in the following table, the rest of the test conditions were the same as in Example 1. After the test was completed, the yield of the crystal form III was the same as that of the product The purity results are shown in the table below:
[0023] solvent
[0024] From the screening of preparation conditions, it can be seen that the composite solvent is superior to single solvent crystallization in terms of product yield and purity.
experiment example 1
[0025] Experimental Example 1 Stability Experiment
[0026] Instrument model: D / Max-RA Japan Rigaku X-ray powder diffractometer
[0027] Rays: monochromatic Cu-Kα rays
[0028] Scanning mode: θ / 2θ, scanning range: 3-45°
[0029] Temperature range: 294K Voltage: 40KV
[0030] The comparison of X-ray diffraction data is shown in Table 1.
[0031] Table 1 X-ray diffraction data comparison table of accelerated stability test samples
[0032]
[0033] Experimental conclusion: after 6 months of accelerated experimentation, the X-ray diffraction spectrum is consistent with the initial data, and no crystal transformation occurs, indicating that the crystal form provided by the present invention has good stability.
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