87597-21-5
87597-21-5 結(jié)構(gòu)式
基本信息
6,8-Dibromoimidazo[1,2-a]pyrazine-ethyl-2-carboxylate
6,8-Dibromo-imidazo[1,2-a]pyrazine-2-carboxylic acid ethyl ester
Imidazo[1,2-a]pyrazine-2-carboxylic acid, 6,8-dibromo-, ethyl ester
物理化學性質(zhì)
制備方法
70-23-5
24241-18-7
87597-21-5
步驟A:制備6,8-二溴咪唑并[1,2-a]吡嗪-2-羧酸乙酯 在室溫下,將2-氨基-3,5-二溴吡嗪(20g,79mmol)溶解于碳酸二甲酯(133mL)中,攪拌至完全溶解。隨后,向反應體系中一次性加入3-溴-2-氧代丙酸乙酯(17.14g,79mmol)。將反應混合物加熱至110℃,持續(xù)攪拌3小時。反應完成后,將混合物冷卻至室溫并繼續(xù)攪拌過夜。向反應混合物中加入水和二氯甲烷(DCM),分離水相并用DCM萃取。合并有機相,用水洗滌后,用無水硫酸鈉(Na2SO4)干燥,過濾并蒸發(fā)溶劑。通過快速柱色譜法純化,得到13.95g(產(chǎn)率50.6%)目標化合物6,8-二溴咪唑并[1,2-a]吡嗪-2-羧酸乙酯。產(chǎn)物經(jīng)1H-NMR(300MHz,CDCl3)表征:δ= 8.30(s,1H),8.27(s,1H),4.48(q,2H),1.43(t,3H)ppm。
參考文獻:
[1] Patent: WO2012/80232, 2012, A1. Location in patent: Page/Page column 36-37
[2] Patent: WO2012/80228, 2012, A1. Location in patent: Page/Page column 42-43
[3] Patent: WO2012/80234, 2012, A1. Location in patent: Page/Page column 45
[4] Patent: WO2012/80236, 2012, A1. Location in patent: Page/Page column 64
[5] Patent: US2013/281460, 2013, A1. Location in patent: Paragraph 0270-0271
