RP-HPLC在(Et4N)2Fe4(SPh)10引发的SRN1反应中的应用研究

摘要

首次采用反相高效液相色谱法(RP-HPLC)直接测定1-溴代萘分别与片呐酮碳负离子和苯乙酮碳负离子在铁硫簇合物(Et4N)2[Fe4(SPh)10]催化引发下的SRN1反应产物3,3-二甲基-1-(1-萘基)-2-丁酮和2-(1-萘基)-1-苯乙酮的含量差异.以甲醇/四氢呋喃/水为流动相,经C18色谱柱分离,在254 nm检测波长下,最低检测限分别为0.004 mg/L和0.011 mg/L,线性方程分别在0.012 mg/L～1.4 mg/L和0.011 mg/L～0.8 mg/L范围内具有良好的线性关系,相关系数分别为0.9999和0.9996.%A new reversed-phase high performance liquid chromatography(RP-HPLC) method was introduced for the determination of 3,3-dimethyl-1-(naphthalene-1-yl)butan-2-one and 2-(naphthalene-1-yl)-1-phenylethanone from the (Et4N)2[Fe4(SPh)10]-stimulated SRN1 reaction,using a mobile phase of methanol/tetrahydrofuran/water (70 : 8 : 22 V/V), (70: 12 : 18 V/V) and a C18-column. UV wavelength of 254 nm is used. The minimum detectable quantities are 0. 004 mg/L and 0. 011 mg/L. The linear ranges are 0. 012 mg/L ～ 1. 4 mg/L and 0. 011 mg/L～0. 8 mg/L. The correlation coefficients are 0. 9999 and 0. 9996. The R. S. Ds were smaller than 1.8%. This determination method is simple, rapid and accurate. The theoretic basis was supplied for study of the SRN1 reaction mechanism.