论文部分内容阅读
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 hydrochloride and p-toluidine as raw materials, through diazotization, coupling reaction of sinomenine azo toluene, namely 1- (p-toluene azo) -7,8- didehydro-4-hydroxy -3,7-dimethoxy-17-methyl-9α, 13α, 14α-morphinan-6-one. The effects of raw materials, reaction temperature, reaction time and pH on the yield of the product were investigated. The experimental results show that under the conditions of the ratio of raw material n (sinomenine hydrochloride): n (p-toluidine) is 1.1:1 (mol / mol), the temperature is 0-5 ℃, the pH is 7 and the reaction time is 4 h, The total yield of the product 76.57%, purity 96.25%. The product was characterized by UV, IR, 1HNMR and MS as the target product.