反应详情

A mixture of 4-Chloro-N-[5-chloro-2-(6-methyl-pyridine-3-carbonyl)-pyridin-3-yl]-N-methoxymethyl-3-trifluoromethyl-benzenesulfonamide (30 mg) in 3 mL of 4M HCl in dioxane and 1 mL of water was refluxed for 3 hours. After cooling to rt the mixture was diluted with water and sodium bicarbonate was added until pH was 9. The mixture was extracted with ethyl acetate, dried and concentrated. The residue was further purified via flash column (70% ethyl acetate in hexane) to afford 9.1 mg of title compound as an off white solid. 1H NMR: (400 MHz, CDCl3) δ 8.97 (m, 1 H), 8.35 (m, 1 H), 8.16-8.13 (m, 2 H), 8.08-8.05 (m, 1 H), 7.93-7.91 (m, 1 H), 7.59-7.57 (m, 1 H), 7.25-7.23 (1 H), 2.63 (s, 3 H). MS: (M+H)/z=490.0.

1. additionwas added until pH was 9
2. extractionThe mixture was extracted with ethyl acetate
3. customdried
4. concentrationconcentrated
5. customThe residue was further purified via flash column (70% ethyl acetate in hexane)