Taltirelin alpha crystal form preparation method
A technology of tatirelin and crystal form, which is applied in the field of medicinal chemistry, can solve the problems of difficult drying and low melting point, and achieve the effects of good stability, high yield and good process stability
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0046] Add 3.0g of tatirelin and 30.0ml of aqueous tetrahydrofuran solution (with a water content of 0.5%) into the reaction flask, raise the temperature to 65±2°C, and stir to dissolve. After dissolution and clarification, keep the temperature at 65±2°C and continue stirring for 10 minutes. Then cool down to 3±2°C in an ice-water bath, during which crystals can be seen to precipitate. Crystallize at 3±2°C for 8 hours. Filter and dry under reduced pressure at 35°C. 2.7 g of white solid was obtained. The yield is 90.0%, the melting point is 68-70°C, and the moisture content is 14.6%. X-ray powder diffraction and differential scanning calorimetry and thermogravimetric analysis test patterns are shown in the attached figure 1 And attached figure 2 .
Embodiment 2
[0048] Add 4.0g of tatirelin and 34ml of tetrahydrofuran aqueous solution (with a water volume fraction of 11.8%) into the reaction flask, raise the temperature to 50±2°C, and stir to dissolve. After dissolution and clarification, keep the temperature at 50±2°C and continue stirring for 10 minutes. Then cool down to 2±2°C in an ice-water bath, during which crystals can be seen to precipitate. Crystallize at 2±2°C for 13 hours. Filter and dry under reduced pressure at 40°C. 3.5 g of white solid was obtained. The yield is 87.5%, the melting point is 67-69°C, and the moisture content is 14.9%. X-ray powder diffraction and differential scanning calorimetry and thermogravimetric analysis test patterns are shown in the attached image 3 And attached Figure 4 .
Embodiment 3
[0050] Add 4.0g of tatirelin and 112ml of tetrahydrofuran aqueous solution (with a water volume fraction of 10.7%) into the reaction flask, raise the temperature to 60±2°C, and stir to dissolve. After dissolution and clarification, keep the temperature at 60±2°C and continue stirring for 10 minutes. Then cool down to 5±2°C in an ice-water bath, during which crystals can be seen to precipitate. Crystallize at 5±2°C for 18 hours. Filter and dry under reduced pressure at 40°C. 3.4 g of white solid was obtained. The yield is 85.0%, the melting point is 67-69°C, and the moisture content is 15.0%. It was detected as α crystal form by X powder diffraction.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More