Crystal form of icotinib phosphate and its use
A technology of icotinib phosphate and crystal form, which can be used in medical preparations containing active ingredients, organic active ingredients, organic chemistry, etc. Different crystalline forms, etc.
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0094] Example 1. Preparation of Form I
[0095] 100g of icotinib hydrochloride was dissolved in a mixed solvent of 300ml of ethanol and 200ml of water. A solution formed by dissolving 11.2 g of sodium hydroxide in 100 ml of water was dropped into the above mixed solution at 60° C. until the pH value was 13. The reaction solution was stirred for 1 hour, cooled to room temperature, and a solid precipitated out. Filter and wash with pure water, and vacuum-dry at a temperature lower than 60°C for 8 hours to obtain 90 g of icotinib.
[0096]
[0097] At room temperature, the icotinib solution and phosphoric acid solution (molar ratio 1:1) were reacted in THF to prepare the No. 1 sample of crystal form I of icotinib phosphate. Specific steps: 10 mg icotinib was dissolved in 1 ml THF, and 18.9 μL phosphoric acid solution was added to 3 ml THF to make a 0.1 mol / L phosphoric acid solution. 0.26ml of 0.1mol / L phosphoric acid solution was added to the icotinib solution, and the re...
Embodiment 2
[0099] Example 2. Preparation of Form I
[0100] The preparation steps and conditions of Form I No. 2 sample are the same as in Example 1, except that the molar ratio of phosphoric acid and icotinib in the reaction solution is changed to 1.5:1.
Embodiment 3
[0101] Example 3. Preparation of Form I
[0102] The preparation steps and conditions of Form I No. 3 sample are the same as in Example 1, except that the molar ratio of phosphoric acid and icotinib in the reaction solution is changed to 2:1.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More 