HRID899134
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
N,N-Dimethylcarbamoyl chloride (3.9 g, 0.0368 mol) was added to a mixture of 4-[3-(2-hydroxyethylamino)propyl]benzonitrile (5 g, 0.025 mol; see step (i) above) and triethylamine (3.7 g, 0.368 mol) in dichloromethane (100 mL) at 0° C. Stirring was then continued at room temperature overnight. The reaction mixture was diluted with water and extracted with dichloromethane. The organic layer was washed with water and brine and dried over sodium sulfate. Solvent evaporation under reduced pressure, followed by purification by column chromatography (using 4% methanol in dichloromethane) yielded 7 g of the sub-title compound as a pale yellow, gummy liquid.
WORKUP
后处理
- extractionextracted with dichloromethane
- washThe organic layer was washed with water and brine
- dry with materialdried over sodium sulfate
- customSolvent evaporation under reduced pressure
- customfollowed by purification by column chromatography (using 4% methanol in dichloromethane)