85333-43-3
85333-43-3 結(jié)構(gòu)式
基本信息
8-氯-2-甲基咪唑并[1,2-A]吡嗪
8-chloro-2-MethyliMidazo[1
8-CHLORO-2-METHYLIMIDAZO[1,2-A]PYRAZINE
8-Chloro-2-MethyliMidazol[1,2-a]pyrazine
Imidazo[1,2-a]pyrazine, 8-chloro-2-methyl-
物理化學(xué)性質(zhì)
制備方法
6863-73-6
78-95-5
85333-43-3
以2-氨基-3-氯吡嗪(48.7 g,375.8 mmol)和氯丙酮(120 mL,1504.5 mmol)為原料,在密封管中避光條件下,于90℃攪拌反應(yīng)16小時(shí)。反應(yīng)完成后,冷卻至室溫,加入乙醚(Et2O),過(guò)濾收集形成的固體產(chǎn)物。用額外的乙醚洗滌固體后,將其懸浮于飽和碳酸鈉溶液中,并用二氯甲烷(DCM)進(jìn)行萃取。分離有機(jī)層,用無(wú)水硫酸鈉(Na2SO4)干燥,過(guò)濾后真空濃縮去除溶劑。粗產(chǎn)物通過(guò)乙醚重結(jié)晶純化,得到中間體4(43.2 g,產(chǎn)率68%)為白色固體,無(wú)需進(jìn)一步純化即可用于后續(xù)反應(yīng)。該中間體的熔點(diǎn)為133.5-138.6℃(采用WRS-2A熔點(diǎn)儀測(cè)定)。
參考文獻(xiàn):
[1] Patent: WO2011/110545, 2011, A1. Location in patent: Page/Page column 73-74
[2] Patent: US2012/329792, 2012, A1. Location in patent: Page/Page column 33-34
[3] Journal of Medicinal Chemistry, 2014, vol. 57, # 10, p. 4196 - 4212
[4] Patent: US2015/203498, 2015, A1. Location in patent: Paragraph 0167; 0168
[5] Patent: WO2016/185342, 2016, A1. Location in patent: Page/Page column 39