Application of 274693-26-4, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 274693-26-4 as follows.
(1) The toluene solution of the previous product left in the 100L glass reactor was cooled to 20 C;(2) stirring was cooled to 20 C 21.409kg of hydrochloric acid and 30.75L of methanol was added to the reaction mixture of the reaction vessel; addition was completed and maintained at 20 C for 4h;(3) TLC (ethyl acetate: isooctane = 1: 1, take the upper organic point plate), FTG-3 raw material point disappears, the reaction is complete; stop stirring,Static stratification, separation of the lower methanol aqueous standby;(4) 500L reactor was added to the lower part of the lower methanol aqueous phase,With stirring, 20% aqueous potassium carbonate was added(14.202 kg of potassium carbonate and 56.81 L of purified water);Finally adjust the pH between 9;(5) adding 30.75L of ethyl acetate with stirring, stirring for 30min;Stop stirring, standing stratification, separation of the lower aqueous phase,The upper organic phase into the PE barrel backup;(6) into the lower aqueous phase reactor, 30.75L of ethyl acetate was added,Stirring 30min; stop stirring, standing stratification, separation of the lower aqueous phase;(7) The two organic phases were combined, added to a 100L glass reactor,30.75L purified water was added with stirring, stirred for 30min; stop stirring, standing stratification, separation of the lower aqueous phase;30.75L of purified water was added to the reaction kettle and stirred for 30 minutes;Stop stirring, stratification, leaving the lower aqueous phase;(8) To the organic phase, 384 g of activated carbon (5% of the amount of active carbon is used as crude product and the crude product is calculated in 100% yield) is heated to 50 C,Stir for 30min;(9) was filtered, the filtrate was evaporated under reduced pressure at 50 C solvent,Steamed until there is no liquid outflow; then add ethyl acetate 6.15L steamIn addition to the solvent, repeat 2 times, until the solid is generated, there is no liquid outflow;(10) To the residue was added 38.40L of ethyl acetate was heated to 60 C dissolved (ethyl acetate was used in an amount of 5 times the volume of the crude product, the crude product in 100% yield); The solution was transferred to a 100L glass reactor, heated To 60 C;(11) 46.08 L isooctane (isooctane in an amount of 1.2 times the volume of ethyl acetate) preheated to 60 C was added with stirring; the addition rate was controlled,Keep the internal temperature above 50 C ,During the process of solid precipitation gradually;(12) is added, cooled to 30 C with stirring, stirred for 1h;(13) and then cooled to 10 C and stirred for 2h;(14) was filtered, the reactor and the filter cake with precooled to 0 ~ 10 C of 7.68L ethyl acetate and 9.22L isooctane mixed solvent leaching;(15) The filter cake was dried under reduced pressure at 60 C for 12h to obtain crude product of ticagrelor, with white or almost white crystalline powder 6.577kg; yield 87%.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,274693-26-4, its application will become more common.
Reference:
Patent; Hunan Tianji Caotang Pharmaceutical Co., Ltd.; Song Taifa; Li Linmei; Xiang Zhongyou; Weng Xiaotao; Xia Zhike; He Yanbo; Suo Chenglin; Peng Fangwei; (13 pag.)CN107337675; (2017); A;,
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