摘要
利用邻羟基苯甲醛、伯胺及碳酸二甲酯等为原料,在温和条件下,采用缩合、亲核取代及水解反应合成了目标化合物邻茴香醛。经过筛选实验研究,确定了合成邻茴香醛的最佳条件为:邻羟基苯甲醛缩正丁胺/二甲基亚砜/KOH/85℃/24 h。与已有文献报道收率60%~70%比较,最大收率达到了81%,通过1HNMR、13CNMR谱及元素分析对产物进行了表征,结果与目标化合物相符。
Using inexpensive and readily available o-hydroxybenzaldehyde ,primary amine and dimethyl carbonate, ortho-anisicaldehyde was synthesized by condensation, nucleophilie substitution and hydrolysis reactions under moderate conditions. Through screening experiments, the optimum synthetic conditions of ortho.hydroxy-benzylidene-butylamine/DMSO/KOH/85 ℃/24 h were established. Compared with reported methods in 60% ~ 70% yields,the maximum yield of 81% was achieved and the method is environmentally friendly. The product was characterized through 1HNMR,13 CNMR spectra and elemental analysis.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2015年第8期951-953,共3页
Fine Chemicals
关键词
邻茴香醛
邻羟基苯甲醛
碳酸二甲酯
表征
精细化工中间体
ortho-anisicaldehyde
o-hydroxybenzaldehyde
dimethylcarhonate
characterization
fine chemical intermediates