67279-23-6
67279-23-6 結(jié)構(gòu)式
基本信息
2,3,5,6,7,8-Hexahydrophthalazine-1,4-dione
1,4-Phthalazinedione,2,3,5,6,7,8-hexahydro-
物理化學(xué)性質(zhì)
制備方法
2426-02-0
67279-23-6
以3,4,5,6-四氫苯酐為原料合成2,3,5,6,7,8-六氫酞嗪-1,4-二酮的一般步驟:將3,4,5,6-四氫鄰苯二甲酸酐(25g,0.164mol)溶于含有三水合乙酸鈉(26.8g,0.197mol)的40%乙酸水溶液(500ml)中,隨后加入水合肼(9.58ml,0.197mol)。將反應(yīng)混合物加熱回流過(guò)夜,然后冷卻至室溫。過(guò)濾收集所得固體產(chǎn)物,依次用水和乙醚洗滌,最后在真空下干燥,得到目標(biāo)化合物2,3,5,6,7,8-六氫酞嗪-1,4-二酮(23g,收率84%)。產(chǎn)物經(jīng)1H NMR(250MHz,d6-DMSO)表征:δ1.64(4H,br s,2×CH2),2.34(4H,br s,2×CH2),11.30(2H,br s,2×NH);質(zhì)譜(ES+)顯示m/e 167 [MH]+。
參考文獻(xiàn):
[1] Patent: US2010/41663, 2010, A1. Location in patent: Page/Page column 42
[2] Patent: WO2008/110611, 2008, A1. Location in patent: Page/Page column 104
[3] Patent: US6255305, 2001, B1
[4] Patent: WO2011/80510, 2011, A1. Location in patent: Page/Page column 71
[5] Journal of Organic Chemistry, 1955, vol. 20, p. 707,708