Thompson W C, Dasgupta A
Department of Pathology, University of New Mexico School of Medicine, Albuquerque 87106.
Clin Chem. 1994 Sep;40(9):1703-6.
We prepared trifluoroacetyl, pentafluoropropyl, and heptafluorobutyl derivatives of amphetamine, methamphetamine, and 3,4-methylenedioxymethamphetamine (MDMA) in 45 s, 1 min, and 6 min, respectively, by using microwave irradiation. Conventional techniques require heating the reaction mixture for 15 min at 40 degrees C for trifluoroacetyl derivatives, 15 min at 75 degrees C for pentafluoropropyl derivatives, and 40 min at 60 degrees C for heptafluorobutyl derivatives. The mass-spectral fragmentation patterns and the gas-chromatographic retention times of the derivatives obtained by both microwave irradiation and conventional heating were similar. Perfluorooctanoyl derivatives of amphetamine can be prepared quantitatively by either heating the reaction mixture for 30 min at 60 degrees C or by 1 min of microwave irradiation. Conversion of methamphetamine and MDMA to the corresponding perfluorooctanoyl derivatives was not quantitative by either technique, although the yield of the derivative in the conventional technique was much higher.
我们通过微波辐射分别在45秒、1分钟和6分钟内制备了苯丙胺、甲基苯丙胺和3,4-亚甲基二氧基甲基苯丙胺(摇头丸)的三氟乙酰基、五氟丙基和七氟丁基衍生物。传统技术制备三氟乙酰基衍生物需要将反应混合物在40℃加热15分钟,制备五氟丙基衍生物需要在75℃加热15分钟,制备七氟丁基衍生物需要在60℃加热40分钟。通过微波辐射和传统加热获得的衍生物的质谱碎裂模式和气相色谱保留时间相似。苯丙胺的全氟辛酰基衍生物可以通过将反应混合物在60℃加热30分钟或通过1分钟的微波辐射定量制备。甲基苯丙胺和摇头丸转化为相应的全氟辛酰基衍生物,两种技术都无法实现定量转化,尽管传统技术中衍生物的产率要高得多。