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用浸渍法制备了Pd(Ⅱ)/γ-Al2O3催化剂。制备了有机锡试剂三丁基苯基锡、三丁基苄基锡、三丁基烯丙基锡,详细考察了影响有机锡试剂和α-卤代酸酯偶联反应的各种因素,得出了反应的最佳条件:有机锡试剂与α-卤代酸的摩尔比为10.4:10,丙酮溶剂最佳用量15mL,反应时间20h,催化剂用量1.5g。结果表明,在有机锡试剂和α-卤代酸酯偶联反应中,钯实际用量很少,对有机锡的摩尔比为8.6×10-3:1。该催化剂有较高的选择性,很高的催化活性,酯基在反应中不被破坏。催化剂可以重复使用,催化剂循环使用5次,偶联反应的产率还很高。用XPS、XRD、电镜等方法对催化剂进行了表征,证明了催化活性中心是金属态的钯。
Pd (Ⅱ) / γ-Al2O3 catalyst was prepared by impregnation method. Preparation of organotin reagent tributyl phenyl tin, tributyl benzyl tin, tributyl allyl tin, a detailed examination of the various factors that affect the organic tin reagent and α-halo acid ester coupling reaction was The reaction conditions were as follows: the molar ratio of organotin reagent to α-halo acid was 10.4: 10, the optimum amount of acetone solvent was 15mL, the reaction time was 20h and the amount of catalyst was 1.5g. The results showed that the actual amount of palladium used in the coupling reaction of organotin reagent and α-halo acid ester was very small, and the molar ratio of organic tin was 8.6 × 10-3: 1. The catalyst has high selectivity, high catalytic activity, ester groups in the reaction is not destroyed. The catalyst can be reused, the catalyst is recycled 5 times, and the yield of the coupling reaction is still very high. The catalysts were characterized by XPS, XRD, SEM and other methods. It was proved that the catalytic activity centers are metalized palladium.