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
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
A solution of 4-methoxyaniline (1.9 g) in dimethylformamide (3 ml) was added dropwise to a solution of carbonyidiimidazole (2.51 g) in dimethylformamide (15 ml) at 0° C. After a reaction time at 0° C. of 15 minutes, the reaction was allowed to continue at room temperature for 45 minutes. Then (2,2-dimethoxyethyl)-(4-phenoxyphenyl)amine (4.1 g) in dimethylformamide (2 ml) was added, and the mixture was heated at 80° C. for 2 hours. After cooling, volatiles were removed and the residue was taken up in ethyl acetate. The organic phase was washed with water and saturated brine. The organic phase was dried over magnesium sulfate and concentrated. The product with the molecular weight of 422.49 (C24H26N2O5); MS (ESI): 423 ([M+H]+), was obtained in this way.
WORKUP
后处理
- waitto continue at room temperature for 45 minutes
- temperatureAfter cooling
- customvolatiles were removed
- washThe organic phase was washed with water and saturated brine
- dry with materialThe organic phase was dried over magnesium sulfate
- concentrationconcentrated
- customMS (ESI): 423 ([M+H]+), was obtained in this way