反应详情

温度

60 °C

Sodium hydride (60% dispersion in mineral oil, 7.5 g, 0.188 mol) was added to a stirred solution of 4-chloro-2-hydroxy-3-nitropyridine (23.68 g, 0.126 mol) in THF (250 mL) at 0° C. After 25 min ethyl bromoacetate (16.7 mL, 0.151 mol) was added and the reaction was warmed to 60° C. After 20 h the reaction was cooled and washed with brine acidified with 1M HCl. The organic layer was dried (Na2SO4) and evaporated in vacuo to a solid which was recrystallised from ethyl acetate/hexanes to give the title compound;

1. temperatureAfter 20 h the reaction was cooled
2. washwashed with brine
3. dry with materialThe organic layer was dried (Na2SO4)
4. customevaporated in vacuo to a solid which
5. customwas recrystallised from ethyl acetate/hexanes