Triethylamine → HCID 86723303, Verbindung

Beteiligte Stoffe

Reaktionsbedingungen

Reaktionsschritte

A mixture of 2-chloro-3-fluoropyridin-4-ylamine (293 mg, 2.0 mmol), 2-chloro-6-fluoro-benzoyl chloride (400 mg, 2.07 mmol) and triethylamine (300 μL, 218 mg, 2.15 mmol) in dioxane (6 mL) was heated at 50° C. for 4 hours. After cooling to ambient temperature, triethylamine (60 μL) and 2-chloro-6-fluorobenzoyl chloride (40 μL) were added. The resultant mixture was heated under reflux for a further 2 hours. The reaction mixture was cooled and concentrated under reduced pressure. The residue was purified by silica gel flash chromatography eluting with DCM and the resultant solid was triturated in diethyl ether, filtered, and dried to give the desired compound as a white solid (380 mg, 63% yield). 1H NMR (400 MHz, DMSO-d6): δ 11.46 (br s, 1H), 8.27-8.23 (m, 2H), 7.59 (td, J=8.3, 6.2 Hz, 1H), 7.47 (d, J=8.1 Hz, 1H), 7.42-7.37 (m, 1H). LCMS (Method C): RT=3.34 min, m/z: 303 [M+H+].

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