Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 866546-07-8, name is 5-Chloro-1H-pyrrolo[2,3-b]pyridine. This compound has unique chemical properties. The synthetic route is as follows. Quality Control of 5-Chloro-1H-pyrrolo[2,3-b]pyridine
[0678] To a stirred solution of 5-chloro-1H-pyrrolo [2, 3-bj pyridine (25 g, 164 mmol) in DMSO (125 mL) at 0 C under an argon atmosphere were added potassium hydroxide (14 g, 246 mmol) and methyl iodide (35 g, 246 mmol). The reaction mixture was warmed to room temperature and stirred for 16 h. After consumption of starting material (by TLC), the reaction mixture was diluted with ice cold water (500 mL) and extracted with EtOAc (2 x 200 mL). The combined organic extracts were dried over sodium sulfate, filtered and concentrated in vacuo to obtain crude. The crude material was purified by column chromatography using 10% EtOAc: Hexane to afford 5-chloro-1-methyl-1H-pyrrolo [2, 3-bj pyridine (22.5 g, 83%) as a pale yellow solid. ?H NMR (CDC13, 500 MHz): 8.28 (s, 1H), 7.88 (s, 1H), 7.22 (s, 1H), 6.41 (s, 1H), 3.89 (s, 3H); LCMS: 90.6%; 166.8 (M+1); (column; Kinetex EVO C-18 (50 x 3.0 mm, 2.6 tm); RT 2.70 mm; mobile phase: 2.5mM NH400CH in water+5% ACN: ACN+5% 2.5mM NH400CH in water; T/B%: 0.01/5, 4/95, 5.5/95; flow rate: 0.8 mL/min) (Gradient); TLC: 20% EtOAc/ Hexane (Rj: 0.6).
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Reference:
Patent; FORUM PHARMACEUTICALS INC.; BURNETT, Duane, A.; BURSAVICH, Matthew, Gregory; HARRISON, Bryce, Alden; (273 pag.)WO2017/31325; (2017); A1;,
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