Dichloromethane → HCID 57932945、化合物

関与物質

反応手順

A CH2Cl2 solution (4 mL) of 8-(1-ethyl-propyl)-2,6-dimethyl-3-(3-methyl-furan-2-yl)-imidazo[1,2-b]pyridazine (32.4 mg, 0.11 mmol) is cooled to 0° C. under a CaSO4 drying tube and treated with NBS (20.1 mg, 0.11 mmol). After 15 minutes at 0° C., the mixture is warmed to room temperature. After an additional 10 minutes, the reaction mixture is poured into H2O (25 mL) and extracted into CH2Cl2 (2×25 mL). The combined organic extracts are washed with aq. brine, dried over Na2SO4, filtered, and concentrated. The crude product is purified by chromatography using hexane-ethyl acetate gradient (100% hexane to 10% ethyl acetate in hexane) to elute the title compound (26.3 mg, 64% yield) as a solid. ES-MS (m/z): calc'd for C18H22BrN3O: 375.1; found 376.2 (M+H); 1H NMR (400 mHz, CDCl3): δ 6.72 (s, 1H), 6.40 (s, 1H), 3.34 (m, 1H), 2.56 (s, 3H), 2.49 (s, 3H), 2.07 (s, 3H), 1.93-1.77 (m, 4H), 0.89 (t, J=7.5 Hz, 6H).

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