Ammonium Hydroxide → HCID 10606940、化合物

反応式

Br[C:2]1[CH:3]=[C:4]([O:8][CH:9]([CH3:11])[CH3:10])[CH:5]=[N:6][CH:7]=1.[OH-].[NH4+:13]>CO.[Cu]Br>[CH:9]([O:8][C:4]1[CH:3]=[C:2]([NH2:13])[CH:7]=[N:6][CH:5]=1)([CH3:11])[CH3:10]

参加物

反応条件

温度: 170 °C

実験手順

Crude 5-bromo-3-isopropoxypyridine (3.71 g, 17.18 mmol) was dissolved in methanol (46 mL) and added to concentrated ammonium hydroxide (29.7%, 14.8 M, 50 mL) and copper(I) bromide (2.46 g, 17.18 mmol) in a heavy-walled glass pressure-tube apparatus. The tube was sealed and the mixture was stirred and heated at 170° C. (oil bath temperature) for 24 h. After cooling, the solution was concentrated by rotary evaporation. Sodium carbonate solution (17.6%, 200 mL) was added, and the mixture was extracted with CH2Cl2 (4×50 mL). The combined CH2Cl2 extracts were dried (MgSO4), filtered, and concentrated by rotary evaporation to give 1.88 g (72.0%) of a brown oil.