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作 者:朱康玲[1] 李美清[1] 李琳[1] 吴方勇[1] 李光兴[1]
出 处:《催化学报》2005年第7期563-566,共4页
摘 要:将新型氯化钴/吡嗪2羧酸钾催化体系用于苄基氯双羰化反应,并对反应条件进行了优化.结果表明,最佳反应条件为氯化钴浓度0.03mol/L,吡嗪2羧酸(Pzca)浓度0.156mol/L,n(Pzca)/n(KOH)=1,n(Ca(OH)2)/n(苄基氯)=2.7,V(1,4二氧六环)/V(H2O)=5,反应温度70℃,CO压力2.0MPa,反应时间10h,此时β苄基α苯丙酮酸的产率为77.3%,双羰化选择性为99.6%.该催化体系能有效地抑制单羰化反应,双羰化反应的选择性和苄基氯转化率都较高.同时对该体系的催化活性体进行了初步解释,并用红外光谱和质谱对产物结构进行了表征.A novel catalytic system CoCl_2/potassium pyrazine-2-carboxylate (KPzca) for double carbonylation of benzyl chloride has been developed. It is very active for the double carbonylation of benzyl chloride at moderate conditions. When the reaction was carried out under the conditions of c(CoCl_2) =0.03 mol/L, c(KPzca) =0.156 mol/L, n(Ca(OH)_2) / n(PhCH_2Cl) =2.7, V(dioxane) / V(H_2O) =5, θ=70 ℃, t=10 h and p=2.0 MPa, the yield of β-benzyl-α-phenylpyruvic acid (BPPA) was 77.3% with the selectivity as high as 99.6%. The single carbonylation reaction was efficiently inhibited in this catalyst system and the majority of the product was BPPA. Thus, the selectivity for BPPA was reasonably high. The structure of the product was characterized by means of IR and MS, and the mechanism of the catalytic reaction was discussed.
关 键 词:吡嗪-2-羧酸钾 钴配合物 苄基氯 双羰化 β-苄基-α-苯丙酮酸
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