3-溴-1,1,1-三氟-2-丙醇辅助CO2与烯丙基缩水甘油醚偶联反应

3-Bromo-1,1,1-trifluoro-2-propanol Assisted Coupling Reaction of CO2 and Allyl Glycidyl Ether

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BTFP与催化剂TBAB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2.0%,TBAB用量为AGE物质的量的2.0%,无需任何反应溶剂,在90℃、0.5 MPa CO2压力下反应18 h,AGC收率可达96.5%。

4-Allyloxymethyl-1,3-dioxolan-2-one（AGC） was prepared via a coupling reaction of allyl glycidyl ether（AGE） and CO2 by using 3-bromo-1,1,1-trifluoro-2-propanol（BTFP） as activator in the presence of a catalytic amount of tetrabutylammonium bromide（TBAB）. The types of quaternary ammonium salts and activators were screened. In addition,the effects of reaction temperature,activator BTFP and catalyzer TBAB dosage,reaction pressure,and reaction time on the yield of product were investigated. A possible reaction mechanism was also proposed. The target product was characterized by gas chromatography coupled to mass spectrometry（GC-MS）,Fourier transform infrared spectroscopy（FTIR）,and nuclear magnetic resonance（NMR）. The results demonstrated that the yield of AGC could reach 96.5% when BTFP dosage was 2.0%（based on the molar mass of AGE,the same below）. TBAB dosage was 2.0%（based on the molar mass of AGE,the same below） at 90 ℃ for 18 h with 0. 5 MPa CO2 without any solvent.