文章摘要
马辉,谷玉杰,王博,赵波,毛伟,吕剑.3-溴-1,1,1-三氟-2-丙醇辅助二氧化碳与烯丙基缩水甘油醚偶联反应研究[J].精细化工,2018,35(6):0
3-溴-1,1,1-三氟-2-丙醇辅助二氧化碳与烯丙基缩水甘油醚偶联反应研究
3-Bromo-1,1,1-trifluoro-2-propanol Assisted Coupling Reaction of CO2 and Allyl Glycidyl Ether
投稿时间:2017-03-25  修订日期:2017-08-13
DOI:
中文关键词: 3-溴-1,1,1-三氟-2-丙醇  二氧化碳  烯丙基缩水甘油醚  4-烯丙氧甲基-1,3-二氧环戊-2-酮  偶联反应
英文关键词: 3-bromo-1,1,1-trifluoro-2-propanol  CO2  allyl glycidyl ether  4-allyloxymethyl-1,3- dioxolan-2-one  coupling reaction
基金项目:陕西省科技统筹创新工程项目
作者单位E-mail
马辉 西安近代化学研究所 huima_204@163.com 
谷玉杰 西安近代化学研究所  
王博 西安近代化学研究所  
赵波 西安近代化学研究所  
毛伟 西安近代化学研究所  
吕剑 西安近代化学研究所  
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中文摘要:
      以烯丙基缩水甘油醚(AGE)、CO2为原料,以3-溴-1,1,1-三氟-2-丙醇(BTFP)为活化剂,以四丁基溴化铵(TBAB)为有机分子催化剂,经偶联反应合成4-烯丙氧甲基-1,3-二氧环戊-2-酮(AGC)。对四丁基季铵盐和活化剂种类进行了筛选,考察了反应温度、活化剂用量、反应压力、反应时间对产物收率的影响,并提出了可能的反应机理。采用GC-MS、FTIR、NMR对目标产物进行了表征。结果表明:BTFP用量为AGE物质的量的2%,TBAB用量为AGE物质的量的2%,无需任何反应溶剂,90 ℃、0.5 MPa CO2压力下反应18h,AGC收率可达96.5%。
英文摘要:
      4-Allyloxymethyl-1,3-dioxolan-2-one (AGC) was prepared by the coupling reaction of allyl glycidyl ether (AGE) and CO2 using 3-bromo-1,1,1-trifluoro-2-propanol (BTFP) as activator. The coupling reaction was catalyzed by TBAB organocatalyst. Many kinds of quaternary ammonium salts and activators were screened. The effects of reaction temperature, activator amount, carbon dioxide pressure and reaction time on the yield of the product were investigated. A possible reaction mechanism was proposed. The product was analyzed by gas chromatography coupled with mass spectrometry (GC-MS), infrared spectroscopy (FTIR) and - nuclear magnetic resonance spectroscopy (1H-NMR, 13C-NMR). The results demonstrated that the yield of the corresponding cyclic carbonate could reach 96.5% when BTFP was 2 mol% of AGE, n-butylammonium bromide (TBAB) was 2 mol% of AGE at 0. 5 MPa CO2, 90 ℃ for 18 h under a solvent-free condition.
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