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. 1780-26-3, name is 2-Methyl-4,6-dichloropyrimidine. A new synthetic method of this compound is introduced below., Safety of 2-Methyl-4,6-dichloropyrimidine
At room temperature,1.50 kg of 2-amino-N-(2-chloro-6-methylphenyl)-5-thiazolamide,1.11kg of 4,6-dichloro-2-methylpyrimidine was added to a 50L reactor.Add 13.35kg of tetrahydrofuran,Nitrogen protection, stirring and cooling to -5 C ~ 10 C,The temperature of the reaction solution is maintained at -5C to 10C, and sodium tert-butoxide solids are added to the reaction solution in several portions.The total amount of tert-butoxide sodium solids is 2.13kg, and the addition method is to feed once every 20-30min.Each time no more than 10% of the total and no more than 200g,After the addition, the reaction liquid is allowed to react at -5C to 10C for 1 to 2 hours.After warming the reaction solution to 10 C ~ 30 C,Stir the reaction solution,To HPLC detection of 2-amino-N-(2-chloro-6-methylphenyl)-5-thiazoleamide/N-(2-chloro-6-methylphenyl)-2-[(6-chloro- The amount of 2-methyl-4-pyrimidinyl)amino]-5-thiazolecarboxamide is less than 1.5%.Cool the reaction solution to -10C to 10C.Dropping hydrochloric acid at a concentration of 4 mol/L,Adjust the system pH to 6 to 7,After dropping, continue stirring at -10C10C for 12h,filter,The filter cake is washed with an appropriate amount of water and methanol.The filter cake is vacuum dried at 50-60C.N-(2-chloro-6-methylphenyl)-2-[(6-chloro-2-methyl-4-pyrimidinyl)amino]-5-thiazolecarboxamide 1.364kg, yield 74.06%;
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Reference:
Patent; Huarun Shuang He Limin Pharmaceutical (Jinan) Co., Ltd.; Qin Yunpeng; Jiang Yang; Gao Hongxu; (12 pag.)CN107089976; (2017); A;,
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