4-氟-2-(苯基炔基)苯甲醛可作为有机合成中间体,用于医药、农药等领域的相关化合物制备。
医药; 农药
合成路线 1(1. 合成:1189207-30-4)
产率:81%
合成条件:With potassium phosphate; palladium diacetate; [5-(diphenylphosphanyl)-9,9-dimethyl-9H-xanthen-4-yl]diphenylphosphane In toluene at 120℃; Schlenk technique; Inert atmosphere
实验步骤:一般步骤:在烘箱干燥的Schlenk管中加入溴代羰基1/8(100.0-204.8mg,0.54mmol),苯乙炔(110.2mg,1.08mmol),Pd(OAc)2(4.8mg,4mol%),xantphos( 在室温下,25毫克,8摩尔%和K3PO4(458毫克,2.16毫摩尔),然后是无水甲苯(1.0毫升) 在N 2气氛下,将反应混合物在120℃下搅拌2-6小时。 通过TLC监测炔烃2和9形成的进展,直到反应完成。 然后,将混合物通过硅藻土过滤并用CH 2 Cl 2洗涤。 减压蒸发溶剂并通过硅胶柱色谱(PE / EtOAc)纯化粗材料,分别得到炔烃2和9(72-91%),为粘性液体/半固体。
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