Preparation of Amorphous Form of Ticagrelor
A ticagrelor, amorphous technology, applied in the direction of organic chemistry, can solve the problems of ticagrelor amorphous, and achieve the effect of good stability and stable and controllable process
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Embodiment 1
[0026] At room temperature, add 500 mg of crude ticagrelor into 30 mL of 1,4-dioxane, heat and stir at 55°C until dissolved. Rotate the above solution at about 50°C to remove about 40% of 1,4-dioxane; then pour the remaining solution into n-hexane (40ml) at about -10°C at one time, stirring at about 300rmp / min, a large amount of solids were precipitated, and filtered after about 5 minutes to obtain 530mg of solids, which weighed 460mg after 10 hours of alkaline drying at 40°C. Get a small amount of sample, use PANalyticalEmpyrean X-ray diffractometer to measure XRD, its X-ray powder diffraction pattern is as follows figure 1 shown.
Embodiment 2
[0028] In reaction vessel 1, 500 mg of crude ticagrelor was added into 20 mL of 1,4-dioxane, and heated to dissolve at 65°C. The above solution was rotated under reduced pressure at about 50°C to remove about 35% of 1,4-dioxane; in reaction vessel 2, n-hexane (40ml) was cooled to about -10°C, and about 5mg was added by Example 3 The freshly prepared ticagrelor is amorphous, and the stirring speed is adjusted to about 400rmp / min; then the remaining solution in reaction vessel 1 is poured into reaction vessel 2 at one time, a large amount of solid is precipitated, and it is filtered after about 5 minutes to obtain 550mg of solid, after 10 hours of alkaline autoclaving at 40°C, weighed 480.22mg of white solid. Get a small amount of solid, use PANalyticalEmpyrean X-ray diffractometer to measure XRD, its X-ray powder diffraction pattern is as follows figure 1 shown.
Embodiment 3
[0029] Example 3 was prepared according to the method disclosed in PCT application WO2014 / 083139
[0030] At 20-25°C, 1g of ticagrelor was dissolved in 10ml of methanol to form a solution, and the formed solution was rotary evaporated under reduced pressure at a vacuum of 5mmHg, and the temperature was controlled at 45-50°C to obtain amorphous ticagrelor.
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