A crystal form of lolatrexex hydrochloride and its preparation method and application
A technology of loratrex hydrochloride and crystal form, which is applied in the field of new crystal forms of compounds, can solve problems such as loratrex hydrochloride that have not yet been seen, achieves stable and mass production, is beneficial to popularization and application, and has good yield Effect
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Embodiment 1
[0041] Example 1 Preparation of crude Lolatrox hydrochloride
[0042] Add 5 g of loratrox to a mixed solution of 10 ml of water and 33 ml of methanol, add 1.0 ml of concentrated hydrochloric acid, and heat to completely dissolve. Tetrahydrofuran was added dropwise to precipitate crystals, and the crude Lolatrox hydrochloride was obtained by filtration after standing for crystallization according to conventional methods. The powder X-ray diffraction pattern is shown in figure 2 .
Embodiment 2
[0043] Example 2 Lolatrox hydrochloride crystal form I and its preparation
[0044] Add 5 g of the crude Lolatrox hydrochloride (prepared in Example 1) into 10 ml of purified water, add 0.25 ml of concentrated hydrochloric acid, and raise the temperature to 60° C. to completely dissolve. The temperature was lowered to 45°C and acetone was added dropwise to precipitate crystals, and the crystals were incubated for 60 minutes. Continue to add acetone dropwise to make the total amount of acetone added twice to 50ml. Cultivate the crystals at 45°C for 60 minutes. Slowly reduce to 20-25℃ under stirring, and cultivate the crystal for 120 minutes. Filter and wash 3 times with 15 ml of 85% acetone aqueous solution. The filter cake was vacuum dried at 35°C to constant weight. Lolatrox hydrochloride crystal form I was obtained with a purity of 99.7% and a yield of 92.6%.
[0045] Such as figure 1 As shown, the crystalline form I of loratrax hydrochloride was determined by powder X-ray d...
Embodiment 3
[0046] Example 3 Lolatrox hydrochloride crystal form I and its preparation
[0047] Add 5 g of the crude Lolatrox hydrochloride (prepared in Example 1 or commercially available raw material) to 7.5 ml of purified water, add 0.1 ml of concentrated hydrochloric acid, and raise the temperature to 50° C. for complete dissolution. The temperature was lowered to 40°C and acetone was added dropwise to precipitate crystals, and the crystals were incubated for 45 minutes. Continue to add acetone dropwise to bring the total amount of acetone added twice to 40ml. Cultivate the crystals at 45°C for 45 minutes. Slowly reduce to 20°C while stirring, and cultivate crystals for 90 minutes. Filter and wash 3 times with 15 ml of 85% acetone aqueous solution. The filter cake was vacuum-dried at 35°C to constant weight to obtain the crystal form I of lolatrox hydrochloride with a purity of 99.6 and a yield of 91%.
[0048] Such as figure 1 As shown, the crystalline form I of loratrax hydrochloride...
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