摘要
本实验在干燥HCl气体催化下,分别进行了辛弗林与甲醇、无水乙醇、异丙醇、叔丁醇、苯甲醇及苯酚反应的研究,并对影响产率的因素(如pH、反应温度、反应时间)进行了优化。结果显示,该方法成功避免了经典的酚羟基烃基化和N-烃基化的副反应,高选择性合成了辛弗林苄基O-甲基化、苄基O-乙基化以及苄基O-苯甲基化目标物,适用于小分子及易于给出电子的伯醇。通过对比实验,在反应体系pH为3,反应温度50℃,反应时间12 h或10 h的优化条件下,产物收率均达85%以上,纯度均达99%以上,结构通过1H-NMR进行表征。
In this experiment, the reaction of synephrine with methanol, absolute ethanol, isopropanol, tert-butanol, benzyl alcohol and phenol were carried out under the catalysis of dry HC1 gas. The factors affecting the yield（ such as pH,reaction temperature and reaction duration） were optimized. The results showed that this method successfully avoided the classical side reactions of phenolic hydroxylation and A^-alkylation, and synthesized benzyl O-methylation, benzyl O-ethylation and benzyl 0-benzene with high selectivi-ty. It was suitable for primary alcohols with small molecule or easy to give electronics. Through the compared experiment, the opti-mum conditions were obtained：the reaction system pH was 3 ,reaction temperature was 50℃ ,reaction duraation was 12 h or 10 h. Under the optimized experimental conditions, the yield of the products were above 85% ,the purity were above 99% and the structure were characterized by 1 H-NMR.
出处
《化学研究与应用》
CAS
CSCD
北大核心
2017年第4期573-576,共4页
Chemical Research and Application
关键词
辛弗林
烃基化
选择性
合成
synephrine
O-alkylation
selectivity
synthesize
