炔丙基丙二酸二甲酯主要用于医药和农药领域的有机合成反应,作为关键中间体参与多种化学反应。
医药; 农药
合成路线 1(1. 合成:95124-07-5)
产率:67%
合成条件:Stage #1: at 0 - 20℃; for 1.25 h; Stage #2: at 0 - 20℃;
实验步骤:一般步骤:在室温下将小Na片(2.30g,100mmol)小心地加入EtOH(100mL)中。在将制备的EtONa溶液冷却至0℃后,在10分钟内将丙二酸二乙酯(16.0g,100mmol)加入到搅拌的溶液中。 15分钟后,将溶液温热至室温并搅拌50分钟。将烯醇化物溶液再冷却至0℃,并在20分钟内加入3-溴丙炔(11.9g,100mmol)。 30分钟后,将溶液温热至室温并搅拌过夜。蒸发反应混合物并用H 2 O洗涤。将水层用Et 2 O萃取两次。将合并的有机层用Na 2 SO 4干燥并蒸发。通过蒸馏和硅胶柱色谱(己烷-AcOEt 10:1)纯化残余油,得到(丙-2-炔基)丙二酸二乙酯(11.9g,60.0mmol),产率60%。该产物也由三乙基十二烷基甲酸盐 - 氧化物和3-溴丙炔制备。 2丙二酸二乙酯(丙-2-炔基):
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