HRID2242217
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of pyridine-2,5-dicarboxylic acid-5-methyl ester (1.0 g, 5.52 mmol), 1,1′-carbonyldiimidazole (0.984 g, 6.07 mmol), 1,2-dichloroethane (30.0 mL) and DMF (8.0 mL) was stirred at room temperature for 1 hour. To the reaction mixture was added N,O-dimethylhydroxylamine hydrochloride (0.535 g, 5.52 mmol) and triethylamine (1.15 mL, 8.28 mmol) and stirred at room temperature for 12 hours. The reaction was diluted with dichloromethane (20.0 mL) and washed with water, 0.5N HCl and saturated NaHCO3, dried (Na2SO4), filtered and concentrated in vacuo to afford the title compound (1.0 g, 81% yield).
WORKUP
后处理
- washwashed with water, 0.5N HCl and saturated NaHCO3
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated in vacuo