在微波辐射及相转移催化剂聚乙二醇-600催化条件下无溶剂法制备大茴香腈的研究

Synthesis of anisonitrile from anisaldehyde under solvent-free conditions with microwave irradiation and phase transfer catalysis of polyethylene glycol 600

以大茴香醛为原料,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大茴香腈。确定的最佳反应条件是：大茴香醛与盐酸羟胺物质的量比为1∶1.4~1∶1.6;对应每mmol大茴香醛,SiO2的用量为0.25~0.30 g;催化剂为n（PEG-600）∶n（Na2CO3-NaOH）=7∶3,彻底研磨后用微波辐射功率为730 W,反应时间为3~4 min,制备效果最佳。在此条件下从大茴香醛制备大茴香腈的平均得率达90.18%。

Under microwave irradiation and phase transfer catalysis of polyethylene glycol 600, anisonitrile was prepared directly from anisaldehyde/NH2OH · HCl in the presence of SiO2/ Na2CO3-NaOH under solvent-free condition in one step. The optimal reaction conditions were as follows： The ratio between anisaldehyde： hydroxylamine chlorohydrate = 1 ： 1.4 - 1 ： 1.6 （molar ratio） ; and the dosage of SiO2 was 0.25 - 0.3 g/retool anisaldehyde. PEG-600 and Na2CO3-NaOH in a molar ratio of 7：3 were ground thoroughly at room temperature, and heated by microwave at a power of 730 W for about 3 ~ 4 minutes prior to being used as the catalyst. Under these conditions, the average yield of anisonitrile from anisaldehyde was up to 90.18%.