With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.1271-42-7,Ferrocenecarboxylic acid,as a common compound, the synthetic route is as follows.
Oxalyl chloride (2 mL) was added to ferrocene carboxylic acid (230 mg, 1 mmol) cooled by ice bath. 5 min after, the cooled bath was removed and the solution was stirred at room temperature for 3 h. Excess of oxalyl chloride was removed under vaccuo. Dichloromethane (4 mL) was added. The mixture obtained was added into a solution of E-4 (130 mg, 0.3 mmol) and pyridine (79 mg, 1 mmol) in dichloromethane (4 mL). The mixture was stirred for 1.5 h and poured in water (40 mL). The compound was extracted with 2 ¡Á 40 mL of dichloromethane and washed with 40 mL of water. The solution was dried over magnesium sulphate, filtered and evaporated. The crude product obtained was purified by flash chromatography with silica gel column using CH2Cl2:petroleum ether 3:1 as an eluent. E-5 was obtained as an orange solid (90 mg, 51% yield).Mp = 148 C (diethyl ether/hexane). Rf: 0.66 (diethyl ether:pentane 1:1). 1H NMR (300 MHz, CDCl3): delta 0.16 and 0.22 (s, s, 6H, 6H, 2 (CH3)2Si); 0.93 (t, 3H, J = 7.4 Hz, CH3); 0.95 and 1.00 (s, s, 6H, 6H, 2 (CH3)3Si); 2.46 (q, 2H, J = 7.4 Hz, CH2); 4.23 (s, 5H, Cp), 4.39 and 4.73 (broad s, broad s, 2H, 2H, C5H4); 6.66 and 6.83 (d, d, 2H, 2H, J = 8.5 Hz, C6H4); 6.81 and 6.97 (d, d, 2H, 2 H, J = 8.5 Hz, C6H4); 7.08 and 7.23 (d, d, 2H, 2H, J = 8.5 Hz, C6H4N). 13C NMR (75.47 MHz, CDCl3): delta -4.4 (CH3Si); 13.6 (CH3); 18.2 and 18.3 (t-BuC); 25.7 (t-Bu); 29.0 (CH2); 68.5 (2 CH, C5H4); 70.2 (Cp); 71.2 (2 CH, C5H4); 118.6, 119.6, 119.7, 130.6, 130.7, 131.6 (6CH, 3 C6H4); 135.4, 135.35, 136.7, 137.3, 139.4, 141.3, 153.8, 154.3 (8 Cq, 3 C6H4 + C=C), 168.2 (CO). IR (CH2Cl2, cm-1): 1671 (CO). MS (EI): 771.24 [M]+, 714.26 [M-tBu]+. Analyse: C45H57FeNO3Si2¡¤H2O cald.: C, 68.42; H, 7.53; N, 1.77. Found: C, 68.15; H, 7.53; N, 1.68., 1271-42-7
The synthetic route of 1271-42-7 has been constantly updated, and we look forward to future research findings.
Reference£º
Conference Paper; Dallagi, Tesnim; Saidi, Mouldi; Vessieres, Anne; Huche, Michel; Jaouen, Gerard; Top, Siden; Journal of Organometallic Chemistry; vol. 734; (2013); p. 69 – 77;,
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