10341-26-1

基本信息
1,4-氧氮雜環(huán)庚-5-酮
1,4-氧代氮雜烷-5-酮
1,4-氧代氮雜烷-5-酮,97%
1,4-Oxaxepan-5-one
Homomorpholin-5-one
HoMoMorpholine-5-one
tetrahydro-1,4-Oxazepin-5(2H)-one
tetrahydro-(2H)-1,4-oxazepin-5-one
1,4-Oxazepin-5(2H)-one, tetrahydro-
物理化學(xué)性質(zhì)
制備方法

61128-73-2

10341-26-1
以二氫-2H-吡喃-4(3H)-酮肟為原料合成1,4-氧氮雜環(huán)庚-5-酮的一般步驟:向含有酮肟(0.01 mol)的四氫呋喃(THF,10 mL)溶液中加入T3P(15 mol%,50%溶于乙酸乙酯中的溶液)。在氮氣保護下,將反應(yīng)混合物加熱回流并攪拌1-4小時。通過薄層色譜(TLC)監(jiān)測反應(yīng)進度,確認反應(yīng)完成后,在減壓條件下移除溶劑。將殘余物用蒸餾水(20 mL)稀釋,隨后用乙酸乙酯(2×20 mL)進行萃取。合并有機相,依次用飽和碳酸氫鈉(NaHCO3)溶液(1×10 mL)和鹽水洗滌。有機相經(jīng)無水硫酸鈉(Na2SO4)干燥后,減壓濃縮,得到高純度的目標酰胺產(chǎn)物。
參考文獻:
[1] Tetrahedron Letters, 2011, vol. 52, # 10, p. 1074 - 1077
[2] Patent: WO2012/101654, 2012, A2. Location in patent: Page/Page column 67-68
[3] Zhurnal Obshchei Khimii, 1955, vol. 25, p. 133,135; engl. Ausg. S. 119, 121
[4] Zhurnal Obshchei Khimii, 1955, vol. 25, p. 133,135; engl. Ausg. S. 119, 121
[5] Bioorganic and Medicinal Chemistry Letters, 2001, vol. 11, # 19, p. 2651 - 2653