摘要
以4-溴-2-甲氧基-5-硝基苯酚和异丙基溴为原料,在NaOH作用下发生羟烷基化反应合成目标化合物1-溴-4-异丙氧基-5-甲氧基-2-硝基苯,通过1HNMR、13CNMR和LC-ESI-MS对其结构进行表征,并对影响收率的主要因素进行考察。确定最佳合成条件为:物料比n(异丙基溴)∶n(4-溴-2-甲氧基-5-硝基苯酚)为2.2∶1、NaOH用量15.0 mmol、反应温度90℃、反应时间3 h,在此条件下,目标化合物收率达到90.4%。该方法可用于化合物2-异丙氧基-1-甲氧基-4-硝基苯和2-异丙氧基-1-甲基-4-硝基苯的合成,收率分别为91.2%和92.8%。
Using 4-bromo-2-methoxy-5-nitrophenol and isopropyl bromide as raw materials,we synthesized 1-bromo-4-isopropoxy-5-methoxy-2-nitrobenzene by hydroxyalkylation reaction in the presence of sodium hydroxide,and characterized its structure by 1HNMR,13CNMR,and LC-ESI-MS.Moreover,we investigated the main factors affecting the yield of target compound.The optimum synthesis conditions are determined as follows:the material ratio n(isopropyl bromide)∶n(4-bromo-2-methoxy-5-nitrophenol) of 2.2∶1,the sodium hydroxide dosage of 15.0 mmol,the reaction temperature of 90 ℃,and the reaction time of 3 h.Under above conditions,the yield of the target compound reaches 90.4%.This method can be applied to the synthesis of 2-isopropoxy-1-methoxy-4-nitrobenzene and 2-isopropoxy-1-methyl-4-nitrobenzene,and the yields of them are 91.2% and 92.8%,respectively.
作者
徐小娜
侯党社
柯苗
李桢
朱周静
XU Xiaona;HOU Dangshe;KE Miao;LI Zhen;ZHU Zhoujing(School of Pharmaceutical&Chemical Engineering,Xianyang Vocational Technical College,Xianyang 712000,China;Collaborative Innovation Center of Green Manufacturing Technology for Traditional Chinese Medicine in Shaanxi Province,School of Pharmacy,Shaanxi Institute of International Trade&Commerce,Xi′an 712046,China)
出处
《化学与生物工程》
CAS
2020年第10期31-34,共4页
Chemistry & Bioengineering
基金
咸阳职业技术学院2020年度科研基金项目(2020KJB02)。
