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作 者:李腾[1] 黄桂兰[1] 袁铃[1] 周世坤[1] 杨旸[1]
机构地区:[1]防化研究院,北京102205
出 处:《化学试剂》2017年第7期708-712,共5页Chemical Reagents
摘 要:以氰化钠、2,2,2-三氟苯乙酮、乙酸酐为原料,通过亲核及酯化反应合成了标题化合物。实验考察了无水四氢呋喃、无水硝基甲烷溶剂对反应的影响,结果表明该反应在四氢呋喃溶剂中常温下即可顺利进行,且副产物较少,产率为76.3%。提纯后的化合物经NMR、HPLC-TOF/MS和GC-EI/MS进行结构表征,并考察了该化合物在不同溶剂中的稳定性及低浓度氰化钠衍生为目标化合物的衍生效率。The compound of 1-cyano-2,2,2-trifluoro-1-phenylethyl acetate was synthesized from the sodium cyanide,2,2,2-trifluoro acetophenone,acetic anhydride via the nucleophilic and esterification reactions.The influence for the synthesis reaction when using the anhydrous nitromethane and anhydrous tetrahydrofuran as reaction solvent was investigated.The results indicated that the reaction could be carried out smoothly and stably in tetrahydrofuran at room temperature and contained fewer by products with the yield of 76.3%.After purification,the structure was confirmed by NMR,HPLC-TOF/MS and GC-EI/MS.The stability of the compound in different solvents and the derivatization efficiency of the low concentration sodium cyanide derivative as the target compound were elucidated.
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