825633-94-1

基本信息
5-碘-3-噠嗪酮
5-碘噠嗪-3(2H)-酮
5-碘-3(2H)-噠嗪酮
5-碘吡噠嗪-3(2H-酮)
5-碘-2,3-二氫噠嗪-3-酮
5-Iodopyridazin-3(2H)-one
5-Iodo-3(2H)-pyridazinone
3(2H)-Pyridazinone, 5-iodo-
5-Iodo-3(2H)-pyridazinone, 95+%
5-Iodo-2,3-dihydropyridazin-3-on
5-Iodo-2,3-dihydropyridazin-3-one
5-Iodo-2,3-dihydropyridazin-3-one ISO 9001:2015 REACH
物理化學(xué)性質(zhì)
制備方法

932-22-9

825633-94-1
以4,5-二氯噠嗪-3(2H)-酮為原料合成5-碘噠嗪-3(2H)-酮的一般步驟:在密封管中,將4,5-二氯噠嗪-3(2H)-酮(10g,60.61mmol)與47%的氫碘酸(75mL)混合,反應(yīng)混合物在150℃下加熱25小時(shí)。反應(yīng)完成后,將混合物過濾,并用去離子水(100mL)洗滌固體。隨后,將固體懸浮于去離子水(200mL)中,加熱至50℃,并在攪拌下緩慢加入硫代硫酸鈉,直至溶液呈現(xiàn)淺棕色并觀察到沉淀形成。將所得混合物過濾,濾液在真空下干燥。得到的棕色固體用預(yù)熱至約78℃的乙醇(200mL)洗滌,再次過濾。將紅色至棕色的濾液真空干燥。最后,將獲得的深棕色固體用二氯甲烷(20mL)研磨,接著用己烷(4×30mL)研磨,并在真空下干燥,得到5-碘-2H-噠嗪-3-酮(8.640g,產(chǎn)率64%),為棕色固體。該產(chǎn)物無需進(jìn)一步純化即可用于后續(xù)反應(yīng)。
參考文獻(xiàn):
[1] Patent: US2009/264434, 2009, A1. Location in patent: Page/Page column 29; 47
[2] Bioorganic and Medicinal Chemistry, 2012, vol. 20, # 12, p. 3880 - 3886
[3] Patent: WO2009/142732, 2009, A2. Location in patent: Page/Page column 65-66
[4] Patent: WO2009/152325, 2009, A1. Location in patent: Page/Page column 208-209
[5] Patent: US2008/27041, 2008, A1. Location in patent: Page/Page column 78