Hydrochloric Acid → HCID 89487978, compound

Participants

Reaction Steps

To a solution of N-[2,6-dibromo-4-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]phenyl]-2-methoxy-N-methyl-3-nitro-benzamide (described above) (0.500 g, 0.612 mmole) in 5 ml isopropanol, under argon atmosphere was added stannous chloride (SnCl2, 0.558 g, 2.94 mmole) followed by concentrated hydrochloric acid (0.250 ml). The suspension was stirred under reflux conditions for 2.25 hours. The mixture was then concentrated under vacuum. The residue was treated with water and the product was extracted twice with ethyl acetate. The combined organic extracts were washed with water and dried over sodium sulfate. Afer removal of the solvent, the residue was purified by flash chromatography over silica gel with a mixture of 15% ethyl acetate and 85% cyclohexane. The title compound was obtained as a yellow oil with a retention time of 1.15 min and a M+H+ mass peak of 581 (LC-MS method 6 described after the tables).

Provenance & Evidence