在无溶剂条件下用微波辐射及相转移催化合成肉桂腈

Microwave Assisted and Phase Transfer Catalsis of Polyethylene Glycol 600 Synthesis of Cinnamonitril from Cinnamaldehyde under Solvent-Free Condition

以肉桂醛为原料,在微波辐射及相转移催化剂聚乙二醇-600催化作用下由SiO2/Na2CO3-NaOH混合碱促进的无溶剂一步法直接制备肉桂腈.确定的最佳反应条件是:肉桂醛与盐酸羟胺摩尔比1:1.4～1:1.6;对应每1mmol肉桂醛,SiO2的用量为0.25～0.30 g;催化剂为PEC-600和Na2<CO3>-NaOH(7:3,摩尔比),彻底研磨后用微波辐射功率为520 W,反应时间为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86.9%.

Under microwave irradiation and phase transfer catalsis of polyethylene glycol 600,cinnamonitril was prepared directly from cinnamaldehyde/NH2OH·HCl in the presence of SiO2/Na2CO3-NaOH under solvent-free condition in one step.The optimal reaction conditions were as follows:cinnamaldehydel∶hydroxylamine chlorhydrate=1∶1.4～1.6(molar ratio);the dosage of SiO2 0.25～0.3 g/mmol anisaldhyde.Using PEG-600 and Na2CO3-NaOH(7∶3,molar ratio) as catalyst,grinding thoroughly at heating by microwave with 520 W power about 5 minutes.Under these conditions,the average yield of cinnamonitril from citronellal was up to 86.9%.