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Оригинальный Лейкарт и на Алюминии

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Реєстрація
12.04.24
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PREPARATION OF AMPHETAMINE 1 FROM P2P 5 VIA THE LEUCKART REACTION36Crude P2P 5 oil (1.66 g, 100 m-%) was mixed with formamide (531 mg, 32 m-%) and formicacid (266 mg, 16 m-%) in a round-bottom flask. The mixture was heated with stirring at150 °C for 5h, after which it was allowed to cool to room temperature and HCL (32%, 8,8ml) was added. The mixture was then refluxed at 110 °C for 2h, after which it was allowedto cool to room temperature, diluted with H2O, made basic with a NaOH-solution,extracted with DCM and dried over MgSO4. Solvents were evaporated to give 1.437 g ofbrown crude amphetamine 1 oil.1H and 13C NMR (CDCl3) was run on the crude product to find characteristic peaks andtentatively identify the main components.7.1.2 PREPARATION OF AMPHETAMINE 1 FROM P2P 5 VIA REDUCTIVE AL/HGCL2 AMINATION74Aluminium foil (1.8 g), EtOH (108 ml) and HgCl2 (332 mg, 1.2 mmol, 1.2 mol-%) was put inround-bottom flask and stirred at 0 °C for 30 min. Crude P2P 5 oil (1.8 g, 13.4 mmol, 100mol-%) and NH3 (2 mol/l, 54 ml, 54 mmol, 400 mol-%) was added into a separate flask at0 °C. The P2P 5 / NH3 solution was added slowly to the aluminium foil / HgCl2 solution at0° C. The mixture was heated to 72 °C, held for 2h with stirring and cooled to roomtemperature, after which it was diluted with a saturated KOH/H2O-solution. Theremaining solid aluminium was filtered, the solution was extracted with CH3Cl2, dried withMgSO4 and concentrated in vacuum to give 1.121 g of yellow crude amphetamine 1 oil.The amphetamine 1 oil was crystallized to amphetamine sulfate, by mixing the oil withacetone in a 1:3 ration, adding a few drops of ~30% H2SO4 and letting the mixture standin an ice bath for 1h. The formed crystals were filtered, washed with cold acetone anddried in a 70 °C oven for 4h.The amphetamine 1 oil was crystallized to amphetamine chloride, by mixing the oil withacetone in a 1:3 ration, adding a 0.1 ml 32% HCl and letting the mixture stand in an icebath for 2h. The formed crystals were filtered, washed with cold acetone and dried in a70 °C oven for 4h.521H and 13C NMR (CDCl3) was run on the crude product to find characteristic peaks andtentatively identify the main components.7.1.3 PREPARATION OF P2P 5 FROM PHENYLACETIC ACID 735A round-bottom flask was flame dried and put under argon atmosphere. Phenylacetic acid7 (6.81 g, 50 mmol, 100 mol-%) was put in the flask, dissolved in acetic anhydride 8 (25ml, 250 mmol, 500 mol-%) and purged with argon gas at room temperature for 15 min.Pyridine (1.86 ml, 25 mmol, 50 mol-%) was added and the mixture was heated to 150 °Cunder stirring. After 20h the reaction was quenched with H2O, allowed to cool to roomtemperature, extracted with ethyl acetate (3 x 50 ml), washed with NaHCO3 (2 x 50 ml)and dried with MgSO4. After concentration in vacuum, 7.473 g of yellow crude P2P 5 oilwas obtained. The crude P2P 5 oil was purified once with flash chromatography (20%EtOAc/Hexane) to give a reference compound, which was used to confirm the presenceof P2P 5 in the crude oils used in the research reactions.1H-NMR (CDCl3): δ = 2.15 (s, 3H), 3.70 (s, 2H), 7.20-7.36 (m, 5H)13C-NMR (CDCl3): δ = 29.4, 51.1, 127.2, 128.9, 129.5, 134.4, 206.5
 
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