未明确提及具体用途
未明确提及具体应用领域
合成路线 1(1. 合成:205877-26-5)
产率:93%
合成条件:With tetrabutyl ammonium fluoride In tetrahydrofuran at 20℃; for 5 h;
实验步骤:将1.0g(2.93mmol)中间体6(1)溶解在10.0mL THF中,在室温下向其中逐渐加入14.64mL(14.64mmol)1.0M四丁基氟化铵的THF溶液,然后搅拌混合物 在室温下保持5小时。 反应结束后,加入50mL蒸馏水,用50mL二氯甲烷萃取3次,得到有机层。 收集有机层并用硫酸镁干燥以蒸发溶剂。 使用硅胶柱色谱法分离纯化残余物,得到730mg(2.78mmol)中间体6(2)(产率:93%)。 使用LC-MS鉴定产生的化合物。 C20H15N:M + 270.12
参考文献:
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合成路线 2(2. 合成:205877-26-5)
产率:77%
合成条件:Stage #1: With potassium tert -butylate In tetrahydrofuran at -78℃; for 2 h; Inert atmosphere Stage #2: at -78 - 20℃; for 21 h; Inert atmosphere
实验步骤:在氩气下使t-BuOK(4当量)溶于干燥的THF(2ml / mmol)中并将溶液冷却至78℃.20分钟后,分批加入1.6当量(溴甲基)三苯基溴化鏻并在氩气下搅拌 持续2小时。 然后缓慢滴加醛8(2.47mmol)或9(0.74mmol)的无水THF(2ml / mmol)溶液,并在78℃下继续搅拌1小时,在室温下搅拌20小时。 将溶液与相同体积的NH 4 Cl(aq)混合,用2M HCl(aq)酸化,并用乙酸乙酯(350ml)萃取。 将有机层用Na 2 SO 4干燥,过滤并真空蒸发溶剂。 在SiO 2柱(20%CHCl 3的己烷溶液)上通过色谱法纯化残余物,得到标题化合物7a(510mg),77%,(黄色固体)或7b(80mg,41%,浅黄色结晶固体;经半色谱分析后) 将固体油状物溶于热己烷中,使溶液达到室温,过滤并真空浓缩。
参考文献:
- [1] Tetrahedron, 2016, vol. 72, # 44, p. 7081 - 7092 [2] Journal of Organic Chemistry, 2010, vol. 75, # 9, p. 3053 - 3068 [3] Journal of Organic Chemistry, 2011, vol. 76, # 21, p. 8726 - 8736