微波条件下SiO_2/K_2CO_3促进的无溶剂法由肉桂醛/NH_2OH·HCl直接制备肉桂腈

Microwave Assisted Synthesis of Cinnamonitrile from Cinnamaldehyde/NH_2OH·HCl Enhanced by SiO_2/K_2CO_3 under Solvent-free Condition

以肉桂醛为原料,在无溶剂的条件下SiO2/K2CO3促进一步法直接制备肉桂腈.确定的最佳反应条件是：当肉桂醛：盐酸羟胺：碳酸钾=1：1.5：0.85（摩尔比）,SiO2用量为每mmol肉桂醛0.3～0.4 g,室温下彻底研磨均匀后,以微波730 W火力加热4～5 min,制备效果最佳.在此条件下从肉桂醛制备肉桂腈的平均得率达90.3%.

Under microwave irradiation, cinnamonitrile was prepared directly from cinnamaldehyde/NH2OH·HCl in the presence of SiO2/K2CO3 under solvent-free condition in one step. The optimal reaction conditions were as follows：cinnamaldehyde ： hydroxylamine chlorhydrate ： potassium carbonate = 1 ： 1.5 ： O. 85 （ molar ratio） ; the dosage of Si02, O. 3 - 0.4 g/mmol cinnamaldehyde; grinding thoroughly at room temperature; and heating by microwave with 730 W power about 4 - 5 minutes. Under these conditions, the average yield of cinnamonitrile from cinnamaldehyde was up to 90.3%.