化学合成。
化学合成
合成路线 1(1. 合成:70138-19-1)
产率:80%
合成条件:Stage #1: With titanium(IV) isopropylate; ammonia In ethanol at 20℃; for 24 h; Inert atmosphere Stage #2: With sodium tetrahydroborate In ethanol for 24 h;
实验步骤:一般步骤:1-(4-(三氟甲基)苯基)乙酮(400mg,2.13mmol),Ti(Oi-Pr)4(1.25mL,类似物.4.25mmol)和氨在EtOH(2M, 将5.30mL,类似物(10.6mmol)在氩气下在室温下搅拌24小时,然后加入NaBH 4(120mg,3.19mmol),并将所得混合物再搅拌24小时。 使用HCl(6M)将反应混合物的pH调节至pH 2,并用叔丁基甲基醚(TBME)(3×20mL)洗涤。 使用NaOH(粒料)将pH调节至约10,并用TBME(6×30mL)萃取混合物。 将合并的有机相用MgSO 4干燥,减压除去溶剂,得到210mg(1.11mmol,52%)黄色油状物。
参考文献:
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