醋酸钯和苯胂酸协同催化苯甲腈水合制备苯甲酰胺

Preparation of Benzamide by Hydration of Benzonitrile with Palladium Acetate and Phenylarsonic Acid as Synergistic Catalyst

以醋酸钯和苯胂酸(物质的量之比nPd∶nAs=3∶2)作为协同催化剂,用于催化苯甲腈水合制备苯甲酰胺。在不额外添加有机溶剂条件下,利用过量苯甲腈兼做溶剂,该反应获得了99%的高产率和100%的苯甲酰胺选择性以及高达186 mol·kg^-1·h^-1的时空收率,循环反应5轮未发现明显的活性与选择性的降低,催化剂具有良好的循环使用性能。产物的结晶分离研究结果表明苯甲酰胺在0 ℃的析出百分比为73%,简单过滤即可收集。

A new catalytic method for benzonitrile hydration in the absence of solvent was developed by using palladium acetate and phenylarsonic acid (molar ratio nPd∶nAs=3∶2) as catalyst, which exhibited high catalytic activity (space-time yield (STY)=186 mol·kg^-1·h^-1) and recyclability. Moreover, the product can be isolated as pure crystals and filtered from the reaction mixture after the reaction system cooling to low temperature (0 ℃), and the product was characterized by 1H NMR, 13C NMR and FT-IR.