HRID1831248
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 N-(6-hydroxy-pyridin-3-yl)-benzamide (0.64 g, 3.00 mmol), N-methyl-N-phenylcarbamoyl chloride (0.51 g, 3.00 mmol) and 1,4-diazabicyclo[2.2.2]octane (0.34 g, 3.00 mmol) in dimethylformamide (15 ml) was stirred at room temperature for 1 hour. Water was added and the precipitates were collected by suction. The solids were dissolved in dichloromethane and the solution was dried over sodium sulphate, filtered and evaporated in vacuo. The residue was dissolved in ethyl acetate and filtered over a short pad of silica. Evaporation of the solvent in vacuo yielded the title compound (0.70 g, 68% yield) as a thick oil.
WORKUP
后处理
- customthe precipitates were collected by suction
- dissolutionThe solids were dissolved in dichloromethane
- dry with materialthe solution was dried over sodium sulphate
- filtrationfiltered
- customevaporated in vacuo
- dissolutionThe residue was dissolved in ethyl acetate
- filtrationfiltered over a short pad of silica
- customEvaporation of the solvent in vacuo