摘要
以咔唑和β-氯乙醇为原料,PEG1000和四丁基碘化铵为相转移催化剂,四氢呋喃或1,4-二氧六环为溶剂,Na2CO3和NaOH作碱,加入0.6 mmol碘化钠或碘化钾,40℃下反应2 h得标题化合物粗品。此粗品通过重结晶得到高纯度的标题化合物,并回收原料,考察了催化剂、碱、溶剂和温度对收率的影响,确定了最佳反应条件,化合物通过熔点和1HNMR进行了表征。
The process has been established for the production of crude 9-(2-ethoxyl) carbazol, with carbazol and β-chloro- ethyl alchohol as reactants,PEG 1000 and tetrabutyl ammoni- um iodide as phase transfer catalyst, ietrahydrofuran or 1,4- dioxanesodium as solvent ,carbonate and sodium hydroxide as base and 0.02 equivalent iodide/potassium iodide, under 40 ℃ for two hours. The crude product was purified via re- crystallization to afford 9-(2-ethoxyl) carbazol with high purity and the unreacted carbazol could be recycled. Some key fac- tors including catalyst, base, solvent and reaction temperature were investigated and the optimum conditions were obtained. Tthe compound was confirmed by melting point and 1 HNMR.
出处
《化学试剂》
CAS
CSCD
北大核心
2014年第5期469-472,共4页
Chemical Reagents