HRID723339

反应详情

EQUATION

反应方程式

HRID 723339 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. waitto continue at room temperature for 45 minutes
  2. temperatureAfter cooling
  3. customvolatiles were removed
  4. washThe organic phase was washed with water and saturated brine
  5. dry with materialThe organic phase was dried over magnesium sulfate
  6. concentrationconcentrated
  7. customMS (ESI): 423 ([M+H]+), was obtained in this way