Extraction of pseudoephedrine from pharmaceutical (Sudafed) tablets.
Pseudoephedrine was extracted from Sudafed tablets using ethanol, ethanol/methanol (90:10% vol/vol) and methylated spirits. The solvents were chosen with reference to the relevant clandestine literature. For each extraction, one Sudafed tablet was crushed using a mortar and pestle and placed in a beaker. The iron oxide coating was removed by repetitive washing with acetone (10 mL in total) until all of the red colour had disappeared. The acetone was removed by filtration and the residue was allowed to dry. The extracting solvent (15 mL) was added to the beaker, which was then covered with aluminum foil and the sample shaken using mechanical agitation for 15 min. The sample was left to settle for one hour at room temperature, and then filtered using gravity filtration. The solvent was evaporated, and the resultant solid collected.
>>>>>>>>Other methods are here<<<<<<<<
Iodine from iodine tinctures.
Iodine tincture (7 mL, 2.5%) and distilled water (7 mL) were combined together and mixed with swirling. Concentrated hydrochloric acid (1 mL) was added dropwise with swirling, followed by hydrogen peroxide (7 mL, 6 % 20 vols). The mixture was poured into a beaker containing distilled water (50 mL) and left to stand for 20 min. The mixture was subsequently filtered using gravity filtration to reveal the iodine crystals.
Extraction of red phosphorous from matchboxes.
Matchbook strikers were cut off from locally purchased KTWO safety matchboxes and soaked in acetone (10 mL). After 30 min, the red phosphorous was scrapped from the strikers, and the paper discarded. The extracted red phosphorous was washed with distilled water and left to dry to a constant weight. The dry red phosphorous was placed in a beaker, and sodium hydroxide solution (20% wt/vol, 20 mL) was added. This solution was placed on a low heat for 2 h. The final product was filtered, washed with distilled water and left to dry to a constant weight.
Synthesis of methylamphetamine using the Moscow and Hypophosphorous routes.
Six batches of methylamphetamine hydrochloride were prepared using each synthetic route for laboratory grade pseudoephedrine and pseudoephedrine extracted from Sudafed tablets as previously described. In the case of the extracted precursor samples, the essential chemicals (iodine and phosphorous), used in the synthesis, were also extracted from tinctures and matchboxes. Twenty-four batches of methylamphetamine hydrochloride were prepared using each route, providing 48 batches in total.
[1] Moscow route:
Pseudoephedrine hydrochloride (2.0 g) was mixed in a round bottom flask (100 mL) together with red phosphorous (0.6 g), iodine (4.0 g) and distilled water (2 mL) and a condenser attached. The mixture was refluxed for 24 h and then allowed to cool. Once cool, the mixture was diluted with an equal volume of water and the red phosphorus filtered out. A few grams of sodium thiosulfate were placed into a beaker, and sodium hydroxide solution (25% wt/vol, 8 mL) added to basify the solution. This was then added to the filtered reaction mixture, and swirled to reveal methylamphetamine free base
As an oil, which floated to the top of the aqueous solution. Toluene (20 mL) was added to extract the methylamphetamine free base. The toluene extract was clear to pale yellow. Anhydrous hydrogen chloride gas was bubbled through to reveal a white precipitate, which was washed with toluene. The solid was dried under high vacuum.
[2] Hypophosphorous route:
Pseudoephedrine hydrochloride (2.0 g) was placed into a round bottom flask (100 mL) and mixed with iodine (4.0 g) and hypophosphorous acid (3.6 mL) and a condenser attached. The mixture was refluxed for 8 h, then allowed to cool. Once cool, the mixture was diluted with an equal volume of water. A few grams of sodium thiosulfate were placed into a beaker, and 25 % sodium hydroxide solution (24 mL) was added to extract the methylamphetamine free base. Extraction and precipitation of the salt was as previously described.
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