摘要
讨论了合成标题产物的两种方法。以丙烯醛为原料,经缩醛化等反应生成β-乙氧基丙烯醛缩二乙醇后,再与苯胺作用来制取的方法操作步骤多,后处理复杂,产率又低。而以丙炔醇为原料,在丁酮介质中,室温下用三氨化铬硫酸溶液氧化成醛后,直接与苯胺反应来制取,反应步骤少,操作简便,总产率达80%。用高效液相色谱仪以甲醇加氯仿(25:75)为流动相,测得二次重结晶的产品纯度为98.9%。
Two methods for synthesis of β-anilino-acroleinanil(Ⅰ)are discussed. Acrolein as raw material yields β-ethoxyacrolein diethylacetal (Ⅱ) by acetalation. Then Ⅱ reacts with aniline to produce Ⅰ. This synthesis procedure is more complicated and the yield of Ⅰ is low. In butanone and at room temperature, propargyl alcohol and chromium trioxide react, and the product reacts with aniline to produce Ⅰ. The procedure is simple and the yield of Ⅰ is high (80%). The purity of Ⅰ is determined by HPLC. The flow phase is methanol and chloroform (25: 75). The result of determination is satisfactory.
关键词
合成
纯度
测定
缩苯胺形成
synthesis
purity
determination
β-anilino-acroleinanil
anil formation
