化学合成。
有机合成; 医药中间体
合成路线 1(1. 合成:85920-63-4)
产率:83%
合成条件:Stage #1: With pyridine In dichloromethane at 0℃; for 0.25 h; Stage #2: at 0 - 20℃; for 3 h;
实验步骤:通用方法:方法A:改编自Srensen等人的方法.14在0℃向Meldrum酸(1当量)的二氯甲烷溶液中逐滴加入吡啶(2当量),并将所得溶液搅拌15分钟。 将相应的酰氯(1当量)加入该反应混合物中。 此后,将反应在0℃下搅拌1.5小时,并在室温下再搅拌1.5小时。 用2M盐酸淬灭反应,并用二氯甲烷萃取。 将合并的有机层用硫酸钠干燥,过滤,并真空浓缩。 通过硅胶色谱法纯化残余物,使用5%至10%乙酸乙酯的己烷溶液,1%乙酸,得到酰基Meldrum酸(11a-e,j,l,p)。
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