Swist M, Wilamowski J, Parczewski A
Department of Analytical Chemistry, Faculty of Chemistry, Jagiellonian University, Ingardena 3, 30-060 Krakow, Poland.
Forensic Sci Int. 2005 Sep 10;152(2-3):175-84. doi: 10.1016/j.forsciint.2004.08.003.
MDMA was prepared by five different synthesis routes, i.e. by dissolving metal reduction (Al/Hg), cyanoborohydride reduction (NaBH(3)CN), borohydride reduction in low temperature (NaBH(4)), Leuckart reaction and safrole bromination. MDP-2-P was prepared by two different synthesis methods, i.e. by isosafrole oxidation and MDP-2-nitropropene reduction. Each of the synthesis routes was repeated three times in order to establish variation in qualitative composition of route specific impurities between different batches. The analysis of impurities in MDP-2-nitropropene, MDP-2-P, bromosafrole and MDMA was performed with GC-MS. GC/MS was used also in the analysis of impurities in starting materials: safrole, isosafrole and piperonal. As a result of our study the way of determination of MDMA synthesis route determination based on qualitative composition of impurities is proposed.
摇头丸通过五种不同的合成路线制备，即通过溶解金属还原法（铝/汞）、氰基硼氢化钠还原法（NaBH(3)CN）、低温硼氢化钠还原法（NaBH(4)）、吕卡特反应和黄樟素溴化法。3,4-亚甲基二氧苯基-2-丙酮（MDP-2-P）通过两种不同的合成方法制备，即异黄樟素氧化法和3,4-亚甲基二氧苯基-2-硝基丙烯还原法。每条合成路线重复三次，以确定不同批次间特定路线杂质的定性组成差异。采用气相色谱-质谱联用仪（GC-MS）对3,4-亚甲基二氧苯基-2-硝基丙烯、3,4-亚甲基二氧苯基-2-丙酮、溴代黄樟素和摇头丸中的杂质进行分析。气相色谱/质谱联用仪也用于分析起始原料黄樟素、异黄樟素和胡椒醛中的杂质。作为我们研究的结果，提出了基于杂质定性组成确定摇头丸合成路线的方法。
