Reference of 113975-22-7, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 113975-22-7, name is 2-Fluoro-3-iodopyridine, molecular formula is C5H3FIN, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
Example 5 – 2,2′-Difluoro-4,4′-diiodo-3,3′-bipyridine (5a) 2-Fluoro-3-iodopyridine (7.80 mmol, 1.74 g) was dissolved in 40 ml of anhydrous THF under nitrogen atmosphere and the solution was cooled in acetone/C02 bath. LDA (1.1 eq., 1.2 M in hexanes-THF, 8.58 mmol, 7.15 ml) was added dropwise. The reaction mixture became yellowish and after stirring for 0.5h it was analyzed by GC/MS. A clean BCHD reaction was confirmed, the mixture was stirred for additional 0.5h and CuCl2 (1.1 eq., 8.58 mmol, 1.15 g) was added in one portion. The yellow reaction mixture became dark blue, then brown red (within 1-2 h) and then light greenish after warm up to room temperature. The reaction mixture was treated with hexanes and water, the organic phase was removed, and the aqueous phase was extracted with hexanes (2 x -20 ml). The combined organic phases were dried over MgS04 and the solvent was removed by rotary evaporation to give greenish- brownish oil which partially solidified on standing. This crude product was purified by column chromatography (200 ml of silica gel, hexanes :CH2C12 mixtures (2: 1, 1 : 1 : and then 1 :2) as eluants). The solvents were removed from combined fractions and the product was obtained as off-white solid (1.04 g, 60.1%). UV-vis (CH2C12) max, nm226, 244, 268. HRMS (EI) calculated for Ci0H4F2I2N2 443.8432; found 443.8417. 1H NMR (CDC13, 400 MHz): delta 8.01 (d, J= 5.2 Hz, 2H), 7.82 (d, J= 5.2 Hz, 2H); 13C{1H} NMR (CDCI3, 100 MHz): delta 159.28 (d, J (C-F) = 242.8 Hz, quaternary C), 148.5 (d, J(C-F) = 15.62 Hz, CH), 132.1 (d, J(C-F) = 4.6 Hz, CH), 125.0 (dd, J (C-F) = 33.4 Hz, 4.1 Hz), 114.5 (d, J(C-F) = 1.7 Hz). Anal. Calc. for Ci0H4F2I2N2: C, 27.05; H, 0.91; N, 6.31. Found: C, 27.52; H, 0.84;
While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 113975-22-7, 2-Fluoro-3-iodopyridine.
Reference:
Patent; GEORGIA TECH RESEARCH CORPORATION; GETMANENKO, Yulia A.; MARDER, Seth; HWANG, Do Kyung; KIPPELEN, Bernard; WO2013/23108; (2013); A1;; ; Patent; GEORGIA TECH RESEARCH CORPORATION; GETMANENKO, Yulia A.; MARDER, Seth; HWANG, Do Kyung; KIPPELEN, Bernard; WO2013/23106; (2013); A1;,
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