25823-52-3
25823-52-3 結(jié)構(gòu)式
基本信息
2,5,6,7-tetrahydrobenzo[1,2]cyclohepta[4,6-d]pyridazin-3-one
6,7-dihydro-2H-benzo[6,7]cyclohepta[1,2-c]pyridazin-3(5H)-one
3H-Benzo[6,7]cyclohepta[1,2-c]pyridazin-3-one, 2,5,6,7-tetrahydro-
物理化學(xué)性質(zhì)
制備方法
25742-87-4
25823-52-3
以4a,5,6,7-四氫-2H-苯并[6,7]環(huán)庚[c]噠嗪-3(4H)-酮(4.7g,22mmol)為起始原料,將其與無(wú)水氯化銅(II)(6g,44mmol)在乙腈(45mL)中混合,回流反應(yīng)2小時(shí)。反應(yīng)完成后,將混合物冷卻至室溫,隨后倒入冰水(200g)中。通過(guò)10%鹽酸溶液(約20mL×2)和冷水(約20mL×2)依次洗滌所得固體。經(jīng)過(guò)冷凍干燥處理,獲得目標(biāo)產(chǎn)物3-氧代-6,7-二氫-5H-苯并[6,7]環(huán)庚并[1,2-c]噠嗪(4.2g,收率90%),為白色固體。產(chǎn)物經(jīng)1H NMR(300MHz,CDCl3)表征:δ 10.80(寬單峰,1H),7.53-7.21(多重峰,4H),6.77(單峰,1H),2.66(三重峰,J = 6.9Hz,2H),2.45(三重峰,J = 6.9Hz,2H),2.14(四重峰,J = 6.9Hz,2H)。LC-MS分析顯示純度為100%,質(zhì)譜(m/e):213(MH+)。
參考文獻(xiàn):
[1] Patent: WO2008/83353, 2008, A1. Location in patent: Page/Page column 126
[2] Patent: WO2008/83367, 2008, A2. Location in patent: Page/Page column 137
[3] Patent: WO2010/5876, 2010, A2. Location in patent: Page/Page column 60-61
[4] Patent: WO2008/83353, 2008, A1. Location in patent: Page/Page column 126-127
[5] Patent: WO2008/83367, 2008, A2. Location in patent: Page/Page column 137-138
