相转移催化合成大茴香腈的研究

Synthesis of Anisonitrile by Base Phase Transfer Catalysis

以5mL(0.04mol)大茴香醛为原料,在95%乙醇中制备大茴香醛肟,进一步在相转移催化剂作用下以甲苯作带水剂使大茴香醛肟脱水生成大茴香腈。优化反应条件为:相转移催化剂类型为十六烷基三甲基溴化铵(HDTMA),其与大茴香醛的用量比(m/m)为0.02,NaOH与大茴香醛的用量比(m/m)以0.08为宜,反应时间为1.5h。在此条件下,从大茴香醛肟到大茴香腈的最高收率达90.7%,并用IR表征了产物的结构。

Synthesis of anisonitrile was carried out from anisaldehyde in the laboratory. Anisaldehyde was tranfered into aldoxime in the presence of 95% ethanol, and then gave anisonitrile using toluene as dehydrant. The optimal reaction conditions were as follow： 0.1 g base phase transfer catalsis cetyhrimethyl ammonium bromide, 0.4-0.5g NaOH and 1.5 h of reaction time. Under these conditions, the highest yield of anisonitrile from aldoxime was up to 90.7%, and the product anisonitrile was characterized by IR.