Electric Literature of 5654-97-7, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 5654-97-7 as follows.
Dried DMSO (6 mL) was heated to 120 C and a solution of 8 (500 mg, 3.7 mmol) and N-bromosuccinimide (690.6 mg, 3.9 mmol) in dry DMSO (2 mL) was added dropwise. The mixture was stirred at 120 C for 30 min, adjusted to pH 5-6 with aqueous NaHCO3 (5%) and extracted with ethyl acetate. The solvent was removed and the residue was purified by column chromatography using ethyl acetate: hexane (3:1) as eluent to afford 9 as a yellow solid (259.2 mg, 1.76 mmol, 65%). 1H NMR (400 MHz, DMSO-d6, delta = 2.49 ppm): 11.6 (s, 1H), 8.38 (dd, 1H, 3JH,H = 3.3 Hz, 4JH,H = 0.9 Hz), 7.87 (dd, 1H, 3JH,H = 5.0 Hz, 4JH,H = 1.1 Hz), 7.01 (dd, 1H, 3JH,H = 4.8 Hz, 4JH,H = 3.5 Hz). 13C-{1H} NMR (150 MHz, DMSO-d6, delta = 39.5 ppm): 183.0, 164.0, 160.0, 155.2, 132.6, 119.0, 112.9. C7H6N2O2. Found: C 56.66, H 2.83, N 18.72; requires: C 56.76, H 2.72, N 18.91.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,5654-97-7, its application will become more common.
Reference:
Article; Cheng, Xinlai; Merz, Karl-Heinz; Vatter, Sandra; Christ, Jochen; Woelfl, Stefan; Eisenbrand, Gerhard; Bioorganic and Medicinal Chemistry; vol. 22; 1; (2014); p. 247 – 255;,
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