HRID2172405

反应详情

EQUATION

反应方程式

HRID 2172405 反应方程式

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Subsequently, 126 g (0.16 mol) of 1,5,8,12-Tetrakis(p-tolylsulfonyl)-1,5,8,12-tetraazadodecane was dissolved in 1500 ml of anhydrous dimethylform amide and then, 7.2 g (0.3 mol) of NaH was slowly added thereto in a nitrogen atmosphere. The mixture was heated for 30 minutes at a temperature of 80° C. 500 ml of dimethylform amide solution in which 129.5 g (0.16 mol) of the 3,6,9-Tris(p-tolylsulfonyl)-3,6,9-triazaundecane-1,11-dimethanesulfonate was dissolved was slowly added to the mixture at a temperature of 80° C. and then left to sit for 30 minutes. The reaction solution was cooled to room temperature, and also, cooled using iced water, and a filtered precipitate was recrystallized with acetone to produce 1,5,8,12,15,18,21-Heptakis(p-tolylsulfonyl)-1,5,8,12,15,18,21-heptaazacyclotricosane.

WORKUP

后处理

  1. additionwas slowly added to the mixture at a temperature of 80° C.
  2. waitleft
  3. temperatureThe reaction solution was cooled to room temperature
  4. temperaturealso, cooled
  5. customa filtered precipitate was recrystallized with acetone