3. Results and discussion
The synthetic methods described here were chosen such that they PLX-4720 could be feasibly performed in a moderately equipped clandestine laboratory. Elaborate product purification techniques were not used so as to mimic the procedures that may be expected in relatively unsophisticated clandestine laboratories. As such, there were some variations in the concentration of organic impurities that were detected across series of repeat synthesises. The products from each step in the reaction pathway were analysed using GC–MS and 1H NMR spectroscopy. Organic impurities were identified based on the fragmentation pattern of their mass spectrum. The identification of heterotrophic organic impurities was also confirmed by 1H NMR spectroscopy when impurities were of a sufficient concentration to produce distinct NMR signals.
3.1. Safrole from catechol
Safrole was synthesised from catechol in three steps: the methylenation of catechol, the bromination of 1,3-benzodioxole and a Grignard reaction using 5-bromo-1,3-benzodioxole and allyl bromide. The gas chromatogram of safrole synthesised from catechol is shown in Fig. 2 and the eight impurities identified unambiguously are listed in Table 1.