Efavirenz I type crystal preparation method
A technology of efavirenz and type I, which is applied in the field of preparing efavirenz type I crystals, and can solve problems such as being unsuitable for industrial production
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
preparation example Construction
[0041] Preparation method of efavirenz type I crystal
[0042] The present invention provides a kind of preparation method of efavirenz type I crystal, comprising steps:
[0043] (1) A solution containing efavirenz is provided, wherein the solvent of the solution is an organic solvent or a mixed solvent composed of an organic solvent and an antisolvent, and the antisolvent is water, C 5-8 Aliphatic or C 5-10 Aromatic hydrocarbons, or combinations thereof;
[0044] Preferably, efavirenz is dissolved in an organic solvent or a mixed solvent composed of an organic solvent and an antisolvent to form an efavirenz-containing solution.
[0045] Preferably, the anti-solvent is selected from the group consisting of water, n-hexane, cyclohexane, n-heptane, or combinations thereof.
[0046] The water used in the present invention is purified water or pure water, such as distilled water or deionized water; preferably water that has been distilled once or twice.
[0047] Preferably, th...
Embodiment 1
[0071] Add 250 g of the raw material efavirenz into a mixed solvent of 1.2 L of ethanol and 1 L of water, and heat to 50° C. to dissolve completely. After the solution was cleared, the temperature was lowered to 35° C., 2.5 g of type I seed crystals were added, and the crystallization was carried out by heat preservation. After the crystals were precipitated, 1.2 L of water was added dropwise. After the dropwise addition, the mixture was incubated for 1 hour. Then the temperature was lowered to about 5° C., and aging was continued for 1 hour. Filter, collect filter cake, get wet product. Polarizing microscope observation and XRPD analysis were carried out on the wet product, and it was identified as type I crystal. The wet product was dried under reduced pressure at 80°C to obtain 247 g of efavirenz type I crystals. After testing, the XRPD pattern is as follows figure 1 As shown, the DSC spectrum is as image 3 As shown, the IR spectrum is as Figure 5 As shown, the pol...
Embodiment 2
[0073] Add 25g of efavirenz raw material into a mixed solvent of 125mL of ethanol and 100mL of water, and heat to 50°C to dissolve completely. After dissolving, lower the temperature to 40°C, add 0.5 g of mixed seed crystals of type I and type V (molar ratio 1:1), and keep warm for crystallization. After the crystals were precipitated, 100 mL of water was added dropwise. After the dropwise addition, the temperature was lowered to about 5° C., and the mixture was kept for aging for 1 hour. Filter, collect filter cake, get wet product. Polarizing microscope observation and XRPD analysis were carried out on the wet product, and it was identified as type I crystal. The wet product was dried under reduced pressure at 80°C to obtain 24.5 g of efavirenz type I crystals. After testing, the XRPD spectrum, DSC spectrum, IR spectrum, and polarizing microscope photos are basically consistent with those of Example 1.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More