反应详情

To a solution of 5-((3,5-dichloropyridin-4-yl)thio)-N-(3-hydroxypropyl)-4-nitrothiophene-2-carboxamide (800 mg, 1.2 mmol) in chloroform (15 mL) was added Dessmartin reagent (611 mg, 1.4 mmol) at 0° C. The resulting reaction mixture was warmed up to ambient temperature and stirred at this temperature for 6 hours. After this time, the reaction mixture was diluted with chloroform and washed with brine and water. The organic layer was separated, dried (Na2SO4) and concentrated. The crude residue was purified by silica gel chromatography using a 97:3 mixture of dichloromethane and methanol as eluent to afford the title product as a solid (430 mg, 89% yield). 1H NMR (400 MHz, d6-DMSO) δ: 9.64 (1H, s), 8.98 (2H, s), 8.91 (1H, m), 8.39 (1H, s), 3.46 (2H, m), 2.66 (2H, m). MS m/z: 404.04, 406.03 [M+H]+.

1. customThe resulting reaction mixture
2. washwashed with brine and water
3. customThe organic layer was separated
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated
6. customThe crude residue was purified by silica gel chromatography
7. additiona 97:3 mixture of dichloromethane and methanol as eluent