无溶剂条件下用微波辐射及相转移催化合成香茅腈

Microwave Irradiation Phase Transfer Catalytic Synthesis of Citronellyl Nitrile from Citronellal under Solvent-free Condition

以香茅醛为原料，在微波辐射及相转移催化剂聚乙二醇一600催化作用下由SiO：／Na。CO。一NaOH混合碱促进的无溶剂一步法直接制备香茅腈。确定的最佳反应条件是：香茅醛与盐酸羟胺摩尔比1：1．4～1：1．6；对应每mmol香茅醛，SiO2的用量为0．25～0．30g；催化剂为PEG-600和Na2CO3-NaOH（7：3，n／n），彻底研磨后用微波辐射功率为730W，反应时间为4～5min，制备效果最佳。在此条件下从香茅醛制备香茅腈的平均得率达85．05％。

Under microwave irradiation and phase transfer catalysis of polyethylene glycol 600, citronellyl nitrile was prepared directly from citronellal/NH2 OH·HCl in the presence of SiO2/Na2 CO3-NaOH under solvent-free condition in one step. The optimal reaction conditions were as follows： citronellal ： hydroxylamine ehlorhydrate=1 ： 1. 4 ～ 1. 6 （molar ratio） ; the dosage of SiO2 was 0.25～0. 3 g/mmol citronellal; PEG-600 and NazCO3-NaOH（7：3, molar ratio） was used as catalyst; the mixture was ground thoroughly under microwave heating with 730 W power about 4 ～5 min. Under these conditions, the average yield of citronellyl nitrile from citronellal was up to 85.05%,