Hydrochloric Acid → 8,9-Di-fluoro-11H-12-thia-6,11-diaza-dibenzo[a,f]azulen-5-ylamine hydrogenchloride

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Reaction Steps

Combine 2-(4,5-difluoro-2-nitro-phenylamino)-benzo[b]thiophene-3-carbonitrile (2.03 g, 6.13 mmol) and Tin(II) chloride (3.49 g, 18.4 mmol) in a mixed solvent of EtOH (20 mL) and 5.0 N HCl (20 mL), heat the suspension to reflux for overnight, cool to RT. The title compound 2.05 g btaine as a yellow solid by suction filtration. 1H NMR (300 MHz, DMSO-d6): δ 11.56 (br, 1H), 10.06 (br, 1H), 9.14 (br, 2H), 7.96-7.85 (m, 1H), 7.71-7.64 (m, 1H), 7.49-7.42 (m, 1H), 7.34-7.29 (m, 1H), 7.22-7.16 (m, 1H), 7.11-7.04 (m, 2H).

Provenance & Evidence