文献类型：期刊文献

中文题名：β-苯胺基丙烯醛缩苯胺的合成与纯度测定

英文题名：Synthesis and Purity Determination of β-Anilino-Acroleinanil

作者：石俊英[1];杨小南[1];李桂贞[2];刘允毅[2];王复[2]

机构：[1]华东化工学院专用化学品研究所;[2]华东化工学院分析测试中心

年份：1992

卷号：18

期号：2

起止页码：232

中文期刊名：华东化工学院学报

外文期刊名：Huadong Huagong Xueyuan xuebao

收录：国家哲学社会科学学术期刊数据库;EI(收录号：1992080551179);Scopus;CSCD:【CSCD2011_2012】；

语种：中文

中文关键词：合成;纯度;测定;缩苯胺形成

外文关键词：synthesis; purity; determination; β-anilino-acroleinanil; anil formation

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.