In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 274693-26-4, name is 2-(((3aR,4S,6R,6aS)-6-(7-(((1R,2S)-2-(3,4-Difluorophenyl)cyclopropyl)amino)-5-(propylthio)-3H-[1,2,3]triazolo[4,5-d]pyrimidin-3-yl)-2,2-dimethyltetrahydro-3aH-cyclopenta[d][1,3]dioxol-4-yl)oxy)ethanol, the common compound, a new synthetic route is introduced below. Formula: C26H32F2N6O4S
a, preparation of crude ticagreride: 56gIsopropyl ticagreIntermediate(0.1 mol, 1.0 eq) was placed in 500 mL of dichloromethane and stirred to dissolve;1.1 g of trifluoroacetic acid (0.01 mol, 0.1 eq) was added dropwise at 0-5 C.The dichloromethane solution was dripped in 30 minutes; after the dropwise addition, the reaction was carried out at 5-10 C.The reaction was monitored by TLC; after 1 hour, TLC showed the reaction of the starting material was completed and 200 mL of water was added.The pH was adjusted to 6-7 with potassium carbonate, and the aqueous layer was extracted with dichloromethane (200 mL×2). The organic phase was combined and then water (300 mL×2).Wash with saturated brine (300 mL × 2), dry over anhydrous sodium sulfate, and filter.Evaporated to dryness under reduced pressure to give 45.8 g of crude ticagrei, yield 88%b, the preparation of ticagrelor amorphous: take 10g crude ticagrei,Placed in 100 ml of tetrahydrofuran solvent, stirred, and warmed to 65-70 C,Maintain this temperature for 30 min, add 1 g of activated carbon, stir for 10 min, filter with hot heat, rinse the filter cake with tetrahydrofuran, and gradually cool the filtrate to 30-35 C with stirring.Then slowly distill off the solvent under reduced pressure, and recycle the tetrahydrofuran.Made a foamy solid, crushed, dried,9.8 g of ticagrelor amorphous product was obtained.Its X-ray powder diffraction pattern is shown in Figure 1.
The synthetic route of 274693-26-4 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Nantong Changyou Pharmaceutical Technology Co., Ltd.; Li Zebiao; Ding Haiming; Zhang Qinghai; Li Keying; Tang Rongjie; Lin Yanfeng; (7 pag.)CN110183436; (2019); A;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia