Novel crystal form of pyrrolidylthiocarbapenem derivative
a technology of pyrrolidylthiocarbapenem and derivative crystals, which is applied in the direction of machines/engines, antibacterial agents, liquid fuel engines, etc., can solve problems such as purity reduction
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Benefits of technology
Problems solved by technology
Method used
Image
Examples
example 1
[0065] (Production Method of Type III Crystal)
[0066] Crude S-4661 (20.0 g) was added to ion-exchanged water (360 ml) and dissolved by heating to about 50 to 55° C., followed by filtration of the solution through a filtering instrument coated with activated carbon (600 mg) while maintaining a temperature of at least 50° C. After the filtrate was cooled to 15 to 20° C., a seed crystal of the type III crystal (20 mg) was put into the solution and stirred for about 120 minutes to deposit a crystal. Further, the crystal was cooled to 0 to 5° C. and aged for 2 hours. Isopropyl alcohol (200 ml) was poured into the solution over about 1 hour. Thereafter, the crystal was further deposited and aged at 0 to 5° C. for 2 hours and further overnight at the same temperature. The crystal was then filtered out. The resultant crystal was washed with 80% isopropyl alcohol water (40 ml), followed by drying under reduced pressure (20 to 30 mmHg) with an aspirator using tap water at room temperature for...
example 2
[0070] (Production Method of Type IV Crystal)
[0071] The type III crystal (5.0 g) obtained in the above-described Example 1 was spread on a glass petri dish, and allowed to stand at 50° C. under reduced pressure (0 to 5 mmHg) for about 7 hours for drying. Thus, type IV crystal (4.8 g) was obtained (recovery rate: 96.0%). A result of powder X-ray diffraction measurement of the resultant crystal is shown in FIG. 2. The diffraction pattern of the resultant crystal in powder X-ray diffraction had main peaks at diffraction angles (2θ)=13.04, 14.98, 15.88, 16.62, 20.62, 21.06, 22.18, 23.90, 26.08, 28.22 and 28.98 (degrees). Further, relatively low peaks were present at diffraction angles (2θ)=23.42, 24.20, 24.46, 27.54, 31.70, 34.14, 34.36, 34.92, 39.82 and 45.24 (degrees).
[0072] Elemental analysis: for C15H24N4O6S2. H2O Theoretical values: C, 41.08, H, 5.98, N, 12.78, S, 14.62 Analytical values: C, 41.01, H, 5.92, N, 12.83, S, 14.56
[0073] Moisture content Theoretical value (monohydrate...
example 3
[0074] (Reproducibility of Production of Type III Crystal)
[0075] A repeat experiment was conducted in order to confirm the reproducibility of the above-described Example 1.
[0076] The diffraction pattern of a resultant type III crystal in powder X-ray diffraction had main peaks at diffraction angles (2θ)=6.62, 13.04, 15.44, 16.58, 17.64, 20.88, 23.26, 25.02 and 25.52 (degrees).
PUM
| Property | Measurement | Unit |
|---|---|---|
| 2θ | aaaaa | aaaaa |
| 2θ | aaaaa | aaaaa |
| 2θ | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More