醛肟的合成及表征研究

Synthesis and Characterization of Aldoxime

以醛2a-2o为原料,分别与盐酸羟胺反应得到了醛肟1a-1o,其中新化合物六种(1d、1e、1f、1j、1l、1o)产物结构经1H NMR和ESI-MS表征确证。并以2-硝基苯甲醛肟(1a)的合成为例,考察了影响反应的主要因素,确定醛肟的合成条件为:物料比n(盐酸羟胺)∶n(2a)=1.2∶1.0,反应溶剂为甲醇,25℃反应5 min。在该条件下,2-硝基苯甲醛肟(1a)收率为90.8%。

A series of aldoxime compounds 1a-1o were prepared from the reaction of aldehydes 2a-2o with hydroxylamine hydrochloride.Among them,1d,1e,1f,1j, 1l and 1o are new compounds.The structures of the products were characterized by^(1)H NMR and ESI-MS.The effect of reaction conditions on the yield of product 1a was investigated as model reaction.The optimal synthesis conditions of compound 1a were as followings:the material ratio of n(hydroxylamine hydrochloride)∶n(2a)=1.2∶1.0,the reaction mixture was stirred in methanol for5 min at 25℃;the yield of 2-nitrobenzaldehyde oxime (1a) was up to 90.8%under the optimal reaction conditions.