化学合成。
化学合成
合成路线 1(1. 合成:134615-22-8)
产率:97%
合成条件:With trans-[OsCl 2 (py){2,6-bis[4’-(S)-isopropyloxazolin-2-yl]pyridine}]; caesium carbonate In isopropyl alcohol at 82℃; for 4 h; Inert atmosphere; Schlenk technique
实验步骤:一般步骤:将催化剂[0.4mol%(配合物12-22)或0.2mol%(双核配合物24)]和酮(2.5mmol)置于干燥氩气氛下的三底Schlenk烧瓶和2-丙醇(45mL)中 ) 加入。 在82℃下搅拌混合物15分钟后,加入5ml 0.06M的2-丙醇(0.3mmol)中的碱(Cs 2 CO 3)溶液。 使用HP-6890设备通过气相色谱监测反应。 在所有情况下检测到相应的醇和酮是唯一的产物。 通过GC用Supelcoβ-DEX 120手性毛细管柱测定转化率和e.e.值。
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合成路线 2(2. 合成:134615-22-8)
产率:89%
合成条件:Stage #1: With chloro(1,3-bis(2,6-di-i-propylphenyl)imidazol-2-ylidene)gold(I); water In methanol at 110℃; for 6 h; Stage #2: With C 26 H 26 ClN 2 O 2 RhS; water; sodium formate In methanol at 30℃; for 5 h;
实验步骤:将3-溴苯乙炔(1mmol),[(IPr)AuCl](6.2mg,1mol%),甲醇(1ml)和水(0.5ml)的溶液依次加入25ml Schlenk反应烧瓶中。 将混合物在110℃反应6小时,然后冷却至室温。[Cp * RhCl [(R,R)-TsDPEN](1.7mg,0.003mmol),水(1.5ml)和甲酸钠(340mg) ,5当量。)加入反应烧瓶中。 将混合物在30℃下进一步反应5小时,然后冷却至室温。 通过旋转蒸发除去溶剂,然后通过柱色谱(展开溶剂:乙酸乙酯/石油醚)获得标题化合物,收率为89%,e.e.percent = 89%
参考文献:
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