反应详情

N-(2-t-Butoxycarbonylaminophenyl)-4-(3-cyanopyridin-2-yl)benzamide (210 mg; prepared as described in Method 1 below), 1,4-dioxane (6.8 ml) and a 4M solution of hydrogen chloride in 1,4-dioxane (6.8 ml) were stirred at ambient temperature for 20 hours. The resultant precipitate was collected by filtration and washed with diethyl ether (3×), suspended in water, basified with a 2M aqueous solution of sodium hydroxide and extracted with dichloromethane. The organic extract was dried over sodium sulfate to afford the title compound as a cream solid (130 mg, 82%); NMR Spectrum: (DMSO-d6) 4.94 (br s, 2H), 6.60 (m, 1H), 6.78 (m, 1H), 6.98 (m, 1H), 7.19 (d, 1H), 7.65 (m, 1H), 7.98 (d, 2H), 8.14 (d, 2H), 8.46 (m, 1H), 8.98 (m, 1H), 9.77 (s, 1H); Mass Spectrum: M+H+ 315.

1. filtrationThe resultant precipitate was collected by filtration
2. washwashed with diethyl ether (3×)
3. extractionextracted with dichloromethane
4. extractionThe organic extract
5. dry with materialwas dried over sodium sulfate