青藤碱偶氮甲苯的合成与表征

Synthesis and characterization of Sinomenine-azo-toluene

以盐酸青藤碱和对甲苯胺为原料,通过重氮化、偶合反应制得青藤碱偶氮甲苯,即1-(对甲苯偶氮基)-7,8-二去氢-4-羟基-3,7-二甲氧基-17-甲基-9α,13α,14α-吗啡烷-6-酮,考察了原料配比、反应温度、反应时间和pH对产物收率的影响。实验结果表明:在原料配比n(盐酸青藤碱)∶n(对甲苯胺)为1.1∶1(mol/mol),温度为0～5℃,pH为7,反应时间4 h条件下,产物的总收率76.57%,纯度96.25%。产物经UV、IR、1HNMR和MS表征为目标产物。

Sinomenine-azo-toluene has been synthesized using hydrochloric sinomenine and p-aminotoluene as material by diazotizing and coupling reaction. Sinomenine-azo-toluene was named 1 - （p-toluene azo） -7,8-didehydro-4-hydroxy-3,7-dimethoxy-17-methylmorphinan-6-one by the systematic nomen- clature. The effects of raw material ratio, reaction temperature, reaction time and pH on the yield of product were investigated. The experimental results showed that under the condition of raw material ratio, reaction temperature, reaction time and pH being 1.1： 1（mol/mol） ,0 -5 ℃ ,7 and 4 h relatively,the yield and the purity of Sinomenine-azo-toluene could reach to 76.57% and 96. 25%. The structure of product was confirmed by UV,IR, 1HNMR and MS characterization.