MDPV är likt kokain när det gäller rus och är relativt lätt att koka för en duktig kemist. Det var en populär RC när den var laglig fram till 2010. jag gissar att det används nu för att säljas som flex kokain.
Citat:
2.2.1. Synthesis of 3,4-methylenedioxypyrovalerone (MDPV; 1-(1,3-benzodioxol-5-yl)-2-(1-pyrrolidinyl)-1-pentanone)
2.2.1.1. 1-Benzo[1,3]dioxol-5-yl-pentan-1-one (2)
To a solution of benzo[1,3]dioxole 1 (30 g, 246 mmol) and pentanoyl chloride (31.5 mL, 266 mmol) in dichloromethane (220 mL) at 3 °C was added tin (IV) chloride (36 mL, 307 mmol) dropwise over 30 min, keeping the temperature < 10 °C. After stirring for an additional 15 min, the reaction mixture was poured into a mixture of concentrated hydrochloric acid (150 mL) and ice (200 g) with vigorous stirring. The layers were separated and the organic layer was washed with water (100 mL). The organic layer was dried over sodium sulfate, filtered and concentrated at reduced pressure. The crude product was purified via flash column chromatography using a silica gel cartridge (330 g), eluting with hexanes/ethyl acetate (99:1 to 95:5) to give the product as a colorless oil (26 g, 51%). 1H NMR (CDCl3) δ 7.55 (dd, J = 8.2, 1.7 Hz, 1H), 7.43 (d, J = 1.8 Hz, 1H), 6.83 (d, J = 8.2 Hz, 1H), 6.02 (s, 2H), 2.87 (t, J = 7.4 Hz, 2H), 1.69 (m, 2H), 1.39 (m, 1H), 0.94 (t, J = 7.3 Hz, 3H). 13C NMR (CDCl3) δ 198.8, 151.7, 148.3, 132.2, 124.4, 108.1, 108.0, 102.0, 38.3, 27.0, 22.7, 14.1 (Fig. 1).
2.2.1.2. 1-Benzo[1,3]dioxol-5-yl-2-bromo-pentan-1-one (3)
To a stirring solution of 1-benzo[1,3]dioxol-5-yl-pentan-1-one 2 (5 g, 24.5 mmol) in acetic acid (15 mL) was added bromine (1.26 mL, 24.5 mmol) dropwise which resulted in a mild exotherm which was kept below 35 °C via water bath. After 1 h at ambient temperature water (50 mL) was added and the mixture was extracted with dichloromethane (2 × 100 mL) and the combined organic layers were concentrated at reduced pressure. The residue was dissolved in dichloromethane (100 mL) and washed with saturated aqueous sodium hydrogen carbonate (75 mL) and the organic layer was concentrated at reduced pressure. The crude product was recovered in quantitative yield and was used without purification in the next step. 1H NMR (CDCl3) δ 7.61 (dd, J = 8.1, 1.7 Hz, 1H), 7.48 (d, J = 1.8 Hz, 1H), 6.87 (d, J = 8.1 Hz, 1H), 6.06 (s, 2H), 5.06 (app t, J = 6.8 Hz, 1H), 2.11 (m, 2H), 1.49 (m, 2H), 0.97 (t, J = 7.2 Hz, 3H).
2.2.1.3. 1-(1,3-Benzodioxol-5-yl)-2-(1-pyrrolidinyl)-1-pentanone hydrochloride (4)
To a stirring solution of pyrrolidine (3.17 mL, 38.6 mmol) in dichloromethane (25 mL) was added 1-benzo[1,3]dioxol-5-yl-2-bromo-pentan-1-one 3 (5 g, 17.5 mmol) in dichloromethane (15 mL) and the resulting solution was stirred at ambient temperature for 16 h. The reaction mixture was diluted with dichloromethane (50 mL), washed with water (50 mL), dried over sodium sulfate, filtered and concentrated at reduced pressure. The crude product was dissolved in 2-propanol (50 mL) and to this stirring solution was added hydrogen chloride (1 N solution in ethyl ether (20 mL) dropwise, producing a white precipitate. After 1 h, the mixture was cooled to 5 °C and filtered. The solid was rinsed with cold 2-propanol (10 mL) and dried to give the hydrochloride salt as a white solid (4.1 g, 75%). 1H NMR (DMSO-d6) δ 10.60 (br s, 1H), 7.76 (dd, J = 8.2, 1.8 Hz, 1H), 7.56 (d, J = 1.8 Hz, 1H), 7.13 (d J = 8.2 Hz), 1H), 6.18 (s, 2H), 5.48 (br q, 6.5 Hz, 1H), 3.59 (m, 1H), 3.39 (m, 1H), 3.20 (m, 1H), 2.98 (m, 1H), 2.10–1.81 (m, 4H), 1.20 (m, 1H), 1.05 (m, 1H), 0.78 (t, J = 7.3 Hz, 3H). 13C NMR (DMSO-d6) δ 195.2, 153.7, 1489.0, 129.9, 126.8, 109.2, 108.5, 67.5, 54.1, 52.6, 32.7, 23.6, 18.2, 14.4.
