反应详情

温度

-20 °C

2-Pyridylcarbinol (7.5 g, 0.069 mole) in dry dimethylformamide (190 ml) was cooled to −20° C. and treated with an 80% dispersion of sodium hydride in mineral oil (2.07 g, 0.069 mole) under argon. The mixture was stirred at −20° C. for two hours. 2-Chloro-5-nitropyridine (8.83 g, 0.058 mole) was added and the mixture was stirred at −20° C. for 0.5 hour then warmed to room temperature and stirred for 18 hours. Water was added dropwise and the solvent removed in vacuo. The residue was dissolved in dichloromethane, washed with 10% aqueous sodium hydroxide solution followed by water, dried (Na2SO4) and evaporated in vacuo to afford the title compound (12.2 g, 91%) as an orange solid.

1. stirringthe mixture was stirred at −20° C. for 0.5 hour
2. temperaturethen warmed to room temperature
3. stirringstirred for 18 hours
4. customthe solvent removed in vacuo
5. dissolutionThe residue was dissolved in dichloromethane
6. washwashed with 10% aqueous sodium hydroxide solution
7. dry with materialdried (Na2SO4)
8. customevaporated in vacuo