Prilocaine crystal form and preparation method thereof
A technology of prilocaine and crystal form, which is applied in the field of prilocaine crystal form and its preparation, can solve the problem of different appearance, solubility, melting point, dissolution rate and biological effectiveness, which affect drug stability, bioavailability and curative effect, Problems such as the crystal form of prilocaine have not been found yet, achieving the effect of low cost, high purity, and simple process route
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Embodiment 1
[0039] Add 100g of crude prilocaine into 600g of n-heptane, stir and heat to 43°C to dissolve completely, stop heating, continue to stir, cool and crystallize, lower the temperature to 0-5°C, keep warm and crystallize for 5h, filter, and dry under reduced pressure at 30°C for 10h Obtained 85.2g refined product, yield: 85.2%, purity (as determined by HPLC): 99.92%, single impurity is less than 0.1%. Carry out XRPD to the obtained refined product, the obtained XRPD pattern is as follows figure 1 As shown, the peak information of its spectrum is shown in Table 1, and the typical TGA graph and DSC graph are shown in figure 2 , and its melting point is 42.00°C (the melting range is 39.81°C-45.49°C according to DSC). The refined product obtained is the prilocaine crystal form of the present application.
[0040] Table 1 Sample powder diffraction data table obtained in Example 1
[0041] 2θ (°) d-value (Å) I / I 0 (%)
Embodiment 2
[0043] Add 1 kg of crude prilocaine into 5 kg of n-hexane, stir and heat to 45°C to dissolve completely, stop heating, continue to stir, cool and crystallize, lower the temperature to 0-5°C, keep warm and crystallize for 5 hours, filter, and dry under reduced pressure at 30°C for 10 hours to obtain 848.6g refined product, yield: 84.9%, purity: 99.91%, single and impurity are less than 0.1%. XRPD was performed on the obtained refined product, and the peak information of the spectrum is shown in Table 2. The refined product obtained is the prilocaine crystal form of the present application.
[0044] Table 2 Example 2 obtained sample powder diffraction data table
[0045] 2θ (°) d-value (Å) I / I 0 (%)
Embodiment 3
[0047] Add 100kg of crude prilocaine into 500kg of n-hexane, stir and heat to 45°C to dissolve completely, stop heating, continue to stir, cool and crystallize, lower the temperature to 0-5°C, heat and crystallize for 5h, filter, and dry under reduced pressure at 30°C for 10h to obtain 85.5kg of refined product, yield: 85.5%, purity: 99.92%, single and impurity are less than 0.1%. XRPD was performed on the obtained refined product, and the peak information of the spectrum is shown in Table 3. The refined product obtained is the prilocaine crystal form of the present application.
[0048] Table 3 Example 3 Gained Sample Powder Diffraction Data Sheet
[0049] 2θ (°) d-value (Å) I / I 0 (%)
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