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Preparation of amorphous ticagrelor

A ticagrelor and amorphous technology, applied in the direction of organic chemistry, can solve the problems of ticagrelor amorphous and other problems, and achieve the effect of good stability and stable and controllable process

Active Publication Date: 2014-12-10
铜陵王燕堂生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] At present, there is no literature report on the precipitation of amorphous ticagrelor directly from the solvent.

Method used

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  • Preparation of amorphous ticagrelor
  • Preparation of amorphous ticagrelor
  • Preparation of amorphous ticagrelor

Examples

Experimental program
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Effect test

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 PANalytical Empyrean 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 PANalytical Empyrean X-ray diffractometer to measure XRD, its X-ray powder diffraction pattern is as follows figure 1 shown.

Embodiment 3

[0029] Example 3 Prepared according to the method disclosed in PCT application WO 2014 / 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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Abstract

The invention provides a preparation method of amorphous ticagrelor. Amorphous ticagrelor is separated out from a solvent for the first time. The process is stable and controllable, and the amorphous ticagrelor prepared by using the method is good in stability.

Description

technical field [0001] The invention relates to the field of solid chemistry, in particular to amorphous ticagrelor and a preparation method thereof. Background technique [0002] Ticagrelor is a new type of selective small molecule anticoagulant. The drug can reversibly act on the purine 2 receptor subtype P2Y12 on vascular smooth muscle cells, has obvious inhibitory effect on platelet aggregation caused by ADP, and takes effect quickly after oral administration, so it can effectively improve the health of patients with acute coronary heart disease. symptom. Its chemical name is (1S,2S,3R,5S)-3-[7-[(1R,2S)-2-(3,4-difluorophenyl)cyclopropylamino]-5-(thiopropyl) -3H-[1,2,3]triazol[4,5-d]pyrimidin-3-yl]-5-(2-hydroxyethoxy)cyclopentane-1,2-diol, its chemical structure As shown in formula (I): [0003] [0004] PCT application WO 200192262 discloses that ticagrelor is amorphous as crystalline form α, and crystalline form α crystallizes into one of crystalline forms I, II,...

Claims

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Application Information

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IPC IPC(8): C07D487/04
CPCC07D487/04
Inventor 许彩霞林玉治
Owner 铜陵王燕堂生物科技有限公司
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