The iron-catalyst compound, name is 1,1′-Dibromoferrocene,cas is 1293-65-8, mainly used in chemical industry, its synthesis route is as follows.
At 78 C, 1.6M n-butyllithium in hexane (1.25 mL) was addeddropwise to a solution of 1,10-dibromoferrocene (0.69 g, 2.0 mmol)in 10 mL THF. The reaction mixture was stirred at the same temperaturefor 0.5 h before adding 2,2,6,6-tetramethylpiperidine(0.40 mL, 2.2 mmol) dropwise. The reaction mixture was stirredfor 3 h, keeping the temperature below 40 C. A solution of tetramethylthiuramdisulfide (0.48 g, 2.0 mmol) in 20 mL THF wasadded, and the reaction mixture was slowly warmed to roomtemperature. After adding water (5 mL), the reaction mixture wasextracted with dichloromethane (2 x 40 mL). The collected organiclayers were washed with water (2 x 20 mL) and dried with anhydroussodium sulfate. After removing the solvent under reducedpressure, the crude product was purified by column chromatography(alumina, dichloromethane/hexane 3:7) to afford P1 as ayellow solid (0.33 g, 43%). 1H NMR (400 MHz, CDCl3): delta 3.18 (s,3H,-N-CH3), 3.54 (s, 3H,-N-CH3), 4.28 (s, 5H, Cp-H), 4.39 (q, 1H,Cp-H, J 1.8 Hz), 4.43 (t, 1H, Cp-H, J 2.8 Hz), 4.76 (q, 1H, Cp-H,J 1.4 Hz). IR (ATR/cm-1): nu 2359, 2342, 1622, 1574, 1508, 1443,1242, 1157, 1107, 1045, 978, 930, 827, 772, 685, 615, 542, 494, 473.
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Reference£º
Article; Horikoshi, Ryo; Sumitani, Ryo; Mochida, Tomoyuki; Journal of Organometallic Chemistry; vol. 900; (2019);,
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