Reference of 288-32-4, These common heterocyclic compound, 288-32-4, name is 1H-Imidazole, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
7kg concentration of 20% sodium hydride DMF solution was taken, while stirring in an ice bath at a rate of 2ml / s, while stirring 7kg 20% imidazole DMF solution was stirred at 60 C for 60min; After cooling with an ice salt bath, 5 kg of 1-chloro-4-(4-chlorophenyl)-2-butanol was slowly added, and the reaction was stirred at 60 C. for 120 min. After cooling with an ice salt bath, the reaction liquid was obtained. To the reaction solution was added 25% by weight of n-hexane, stirred at a rate of 3 revolutions per second for 15 minutes, and then added with ice water of 350% by weight of the reaction solution and stirred at 3 revolutions per second. After precipitation is stopped, the precipitate is filtered, and the cake is washed once with water that is 1/3 times the weight of the cake, and is dried at a rotation speed of 2825 r/min for 60 min, which is 2.5 times and 0.05 times the weight of the product obtained by the centrifugal drying, respectively. Ethyl acetate and activated carbon, After recrystallization at -5C for 13 hours, the recrystallized product was dried at 50C to obtain 1-(2-hydroxy-4-(4-chlorophenyl)butyl)-1H-imidazole. The purity is 99.31%. The 1-(2-hydroxy-4-(4-chlorophenyl)butyl)-1-hydro-imidazole was used as a raw material in Example 6.
The synthetic route of 288-32-4 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Zhuzhou Qianjin Pharmaceutical Co., Ltd.; Peng Kaifeng; Wen Fengqiu; Bai Lu; Li Sanxin; Gong Yun; Li Fujun; (12 pag.)CN105198816; (2018); B;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem