Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 130049-82-0, name is 3-(2-Chloroethyl)-6,7,8,9-tetrahydro-9-hydroxy-2-methyl-4H-pyrido[1,2-a]pyrimidine-4-one. A new synthetic method of this compound is introduced below., COA of Formula: C11H15ClN2O2
(II) hydrochloride (48.77 g, 0.195 mol), (III) (48.54 g, 0.2 mol)(50.4 g, 0.6 mol), potassium iodide (3.3 g, 0.02 mol), 400 mL of acetonitrile and 100 mL of water were heated to 65 G in a 1000 mL three-necked flask and stopped for 16 h reaction. Cooling to 25 G, slowly add lOOmL of water to the system, a large number of solid material precipitation, stirring 30 min, the filter to get crude, filter cake with acetonitrile and water were washed solid, dryingOf crude 72.0 g.The crude product of 72.0 g of (I) was placed in 720 mL of water at a temperature of 20-25 C, 16.8 mL of concentrated hydrochloric acid was added, stirred to form (I) hydrochloride, and the aqueous solution of (I) was washed with 500 mL of dichloromethane 2 times, take the aqueous solution layer, add 7.2g activated carbon decolorization, heating to 50 e, stirring 30min, the filter (I) hydrochloric acid solution.The aqueous solution of (I) salt was cooled to 0-10 C and 500 mL of isopropyl alcohol was added to the system at a temperature of 0-10 C,A solution of 20% sodium hydroxide was slowly added with stirring to adjust the pH of the system to 8-9 to give (I) as a white solid. After the dropwise addition, the mixture was stirred at this temperature for 1 hour and filtered to obtain a solid material. Isopropyl alcohol and water (100 mL + 100 mL), and the resulting solid was (I), about 55.0 g.The above-obtained (I) was added to a mixed solvent of 1100 mL of ethanol and 333 mL of water and heated to reflux to a solid materialDissolved in the lh, slowly cooled to 0-5 e, stirring at this temperature for 16h, to obtain a white solid crystalline material, filtration, to obtain high purity (I), drying to get the product 49.2g, yield 60 %.
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Reference:
Patent; JIANGSU CHIATAI QINGJIANG PHARMACEUTICAL CO LTD (CTQJ); WANG, WUWEI; CHEN, JIE; WU, TINGZHAO; GU, HAICHENG; HE, JIA; (7 pag.)CN103214485; (2016); B;,
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