HRID263536

反应详情

EQUATION

反应方程式

HRID 263536 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

60% Sodium hydride (0.41 g) and 1.71 g of benzyloxyurea were added to 20 ml of dimethylformamide and the mixture was stirred at 80° C. for 7.5 hours. 1,4-Bis(4-chloromethylphenoxy)butane (1.74 g) was added to the reaction mixture at room temperature and the mixture was stirred at 95° C. for 0.5 hour. The reaction product was cooled to room temperature, poured into ice water, mixed with 1N hydrochloric acid and then extracted with ethyl acetate. The organic layer was washed with water and saturated sodium chloride aqueous solution in that order and dried over anhydrous magnesium sulfate and then the solvent was evaporated under a reduced pressure. The resulting crude product was washed with ethyl acetate to obtain 1.94 g of 1,4-bis[4-[(1-benzyloxyureido)methyl]phenoxy]butane.

WORKUP

后处理

  1. stirringthe mixture was stirred at 95° C. for 0.5 hour
  2. temperatureThe reaction product was cooled to room temperature
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with water and saturated sodium chloride aqueous solution in that order
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customthe solvent was evaporated under a reduced pressure
  7. washThe resulting crude product was washed with ethyl acetate