Crystal form of icotinib maleate and its use
A technology of icotinib and maleic acid, which is applied in the field of treatment of cancer and cancer-related diseases, can solve problems such as the impossibility of predicting the crystal structure and properties, and the inability to predict the formation of different crystal forms of organic pharmaceutical compounds
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Embodiment 1
[0065] Example 1. Preparation of Form I (the first preparation method of Form I)
[0066] 100g of icotinib hydrochloride was dissolved in a mixture of 300ml of ethanol and 200ml of water. A solution prepared by dissolving 11.2 g of sodium hydroxide in 100 ml of water was added dropwise to the solution of icotinib hydrochloride at 60° C. until the pH value of the resulting reaction solution reached 13. The reaction solution was stirred for 1 hour and cooled to room temperature to form a precipitate. The precipitate was filtered out, washed with pure water, and dried under vacuum at a temperature lower than 60° C. for 8 hours to obtain 90 g of icotinib.
[0067]
[0068]Form I of icotinib maleate was obtained by reacting icotinib solution with maleic acid solution (1:1 molar ratio) in tetrahydrofuran (THF) at room temperature. Specifically, 10 mg of icotinib was first dissolved in 1 ml of THF to obtain an icotinib solution. In addition, 34.82 mg of maleic acid was also dis...
Embodiment 2
[0070] Example 2. Preparation of Form I
[0071] The second example of the preparation method of Form I is by changing the molar ratio of maleic acid and icotinib in the reaction mixture to 2:1 and following the same steps as described in Example 1 and keeping the same reaction conditions preparation. The melting point of this crystalline form is 173-176°C.
Embodiment 3
[0072] Example 3. Preparation of Form I
[0073] A third example of a preparation method for Form I is by changing the molar ratio of maleic acid and icotinib in the reaction mixture to 1.5:1 (i.e., 3:2) and following the same procedure as described in Example 1. Steps and keep the same reaction conditions for the preparation. The melting point of this crystalline form is 173-176°C.
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Abstract
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