A kind of lycomycin crystal form I and its preparation method and application
A lycomycin and crystal form technology, applied in the field of medicinal chemistry, can solve the problems affecting stability, bioavailability and curative effect, solubility, melting point, dissolution bioavailability, etc., and achieves low equipment requirements and stability. Good, pure and high content
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[0040] The method for preparing lycomycin crystal form I as described in the first aspect of the present invention according to the second aspect of the present invention comprises the following steps:
[0041] S1, after adding acetone to lycomycin, stir and filter with suction to obtain the first filter cake;
[0042] S2, after adding ether and acetone to the first filter cake, heating, cooling, and suction filtration to obtain a second filter cake;
[0043] S3, washing and drying the second filter cake to obtain lycomycin crystal form I.
[0044] In some embodiments of the present invention, in step S1, 2-5 mL of acetone is added to each claricomycin.
[0045] In other embodiments of the present invention, in step S1, the stirring is performed at 20-30° C.; the stirring time is 1.0-1.5 h.
[0046] In some embodiments of the present invention, in step S2, 3-6 mL of ether and 1-2 mL of acetone are added to each gram of the first filter cake.
[0047] In other embodiments of...
Embodiment 1
[0060] Take 10 g of crude lycomycin, add 30 mL of acetone, stir at 25° C. for 1.0 h, and filter with suction to obtain the first filter cake. Add 40 mL of ether and 15 mL of acetone to the first filter cake, heat under reflux at 50° C. for 1.0 h, stop heating, cool to 25° C. with stirring, and suction filter to obtain the second filter cake. Add 10 mL of diethyl ether, wash the second filter cake, and blow dry at 50°C for 4 hours to obtain a white crystalline powder, which is lycomycin crystal form I, with a content of 98.3% and a yield of 80%.
[0061] The diffraction pattern of lycomycin crystal form I was determined by Bruker D8 ADVANCE X-ray powder diffractometer. Test conditions: CuKa 40kv 40mA, divergence slit 1.0mm, solar slit 0.4°; scanning method: continuous scanning; scanning step: 0.02°; scanning range: 3°-45°; scanning speed: 8° / min ; Detector: LynxEye. The result is as figure 1 As shown, the values of the characteristic peaks in the figure are shown in Table ...
Embodiment 2
[0069] Take 10 g of crude lycomycin, add 20 mL of acetone, stir at 25° C. for 1.0 h, and filter with suction to obtain the first filter cake. Add 30 mL of ether and 10 mL of acetone to the first filter cake, heat under reflux at 50° C. for 1.0 h, stop heating, cool to 25° C. with stirring, and suction filter to obtain the second filter cake. Add 10 mL of diethyl ether, wash the second filter cake, and blow dry at 50° C. for 4 hours to obtain a white crystalline powder, lycomycin crystal form I, with a content of 97.6% and a yield of 83%.
[0070]Using the same method as in Example 1 to carry out X-ray powder diffraction detection of lycomycin crystal form I, the lycomycin crystal form I prepared in Example 2 and the lycomycin crystal form I prepared in Example 1 diffractogram They are basically the same, and there are characteristic absorption peaks at diffraction angles 2θ of 5.352°, 7.775°, 8.156°, 10.264°, 10.703°, 15.429°, and 16.652°, indicating that this method can be re...
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