微波辐射及聚乙二醇-600催化条件下无溶剂法制备柠檬腈

Synthesis of Lemonile from Citral Under Microwave Assisted Solvent-free Condition with Phase Transfer Catalysis of Polyethylene Glycol 600

以柠檬醛为原料,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柠檬腈。确定的最佳反应条件是：n（柠檬醛）∶n（盐酸羟胺）=1∶（1.6～1.8）;对应每mmol柠檬醛,SiO2的用量为0.20～0.25 g;催化剂为m（PEG-600）/m（柠檬醛）=0.08,磨细后用功率为520W的微波辐射,反应4 min。在此条件下,从柠檬醛制备柠檬腈的平均产率达90.7%。

Under microwave irradiation and phase transfer catalysis of polyethylene glycol 600, lemonile was prepared directly from citral/NH2OH · HCl in the presence of SiO2/Na2CO3-NaOH under solventfree condition in one step. The optimal reaction conditions were ： n （ citral ） ： n （ hydroxylamine hydrochloride） = 1： （ 1.6 - 1.8 ）, the dosage of SiO2 0. 25 - 0. 3 g/mmol citral, using PEG - 600 as catalyst, m （ polyethylene glycol 600 ）/m （citral） = 0. 08, grinding thoroughly and heating by microwave of 520 W power about 4 minutes. Under these conditions, the average yield of lemonile from citral was up to 90. 7%.