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2,4-Dibromo-5-nitropyridine (1); [0086] 2,4-Dibromo-5-nitropyridine (1) was prepared in two steps from the commercially available <strong>[31872-62-5]4-methoxy-3-nitropyridine</strong> according to the method reported by the literature.1 LC-MS: Rt 6.23 min, m/e 282.7; 1H NMR (CDCl3) delta 8.82 (s, 1 H), 7.96 (s, 1 H).
To a stirred solution of compound D.I (500 mg, 1.77 mmol) in AcOH (20 ml), was added iron powder (400 mg, 7.27 mmol). The reaction mixture was heated at 60 C for 2 hr. After completion of the starting material (by TLC), the reaction mixture was filtered on celite bed and washed with ethyl acetate. The filtrate was concentrated under reduced pressure, and the crude material was diluted with NaHCO3 solution (100 ml) and extracted with ethyl acetate (3x 20 ml). The combined organic extracts was washed with water and dried over anhydrous sodium sulphate, concentrated under reduced pressure to afford compound 208.1 (350 mg, 78.47%, crude) as brown solid, which was used for the next step any further purification. 1H-NMR (CDCl3, 500 MHz) delta 7.94 (s, 1H), 7.54 (s, H), 7.26 (s, 1H), 3.50 (bs, 2H); LCMS m/z = 259 [M+l]. [00268] Synthesis of Compound 208.2.
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