Genistein salt, crystal and preparation method thereof
A genistein and crystal technology, applied in the direction of organic chemistry and the like, can solve the problems of poor water solubility and low bioavailability of genistein, and achieve good solubility and dissolution rate, simple preparation method, and excellent clinical application. Foreground effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0038] Synthesis of genistein sodium salt crystal as shown in formula I: put 100g (0.370mol) genistein into the reaction kettle, add 4L 1,4-dioxane, and heat to dissolve at 75°C , adding an aqueous solution of sodium hydroxide (sodium hydroxide 14.80g, namely 0.370mol, water 370mL), constant temperature, stirring at 100rpm for 2h, cooling down to room temperature at a cooling rate of 5°C / h, crystals were precipitated, filtered, and 1,4- After washing with dioxane and vacuum drying at 45° C. for 24 h, a white solid, namely genistein sodium salt crystal, was obtained with a yield of 87%.
Embodiment 2
[0040] Synthesis of genistein sodium salt crystal as shown in formula I: put 100g (0.370mol) genistein into the reaction kettle, add 4L dimethylacetamide, heat to dissolve at 75°C, add hydrogen Aqueous solution of sodium oxide (sodium hydroxide 17.76g, namely 0.444mol, water 444mL), constant temperature, stirring at 300rpm for 15min, cooling down to room temperature at a cooling rate of 2°C / h, crystals precipitated, filtered, washed with ethyl acetate, 45°C After vacuum drying for 24 hours, a white solid, genistein sodium salt crystal, was obtained with a yield of 90%. The particle size of the obtained crystal is 500 μm, and the crystal is pulverized into seed crystals with different particle sizes of 10 μm, 30 μm, 50 μm, 100 μm, 300 μm, etc. by a ball mill for use in the following examples.
Embodiment 3
[0042] Synthesis of genistein sodium salt crystal as shown in formula I: put 100g (0.370mol) genistein into the reaction kettle, add 4L dimethyl sulfoxide, heat to dissolve at 180°C, add hydroxide Sodium aqueous solution (sodium hydroxide 17.76g, namely 0.444mol, water 444mL), constant temperature, stirring at 200rpm for 15min, cooling down to 120℃ at a cooling rate of 5℃ / h, throwing in 10μm seed crystals (0.1094g, uniform Suspended in 100mL water, the seed crystals account for 0.1022% of the theoretical yield of genistein sodium salt crystals), dropped to 4°C with a cooling rate of 5°C / h, crystals were precipitated, filtered, washed with isopropanol, 45 After vacuum drying at °C for 24 hours, a white solid, genistein sodium salt crystal, was obtained with a yield of 93%.
PUM
| Property | Measurement | Unit |
|---|---|---|
| particle diameter | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More