反応 #1929018

反応方程式

water

diethylenetriamine

p-toluenesulfonyl chloride

→

desired product

tris(p-toluenesulfonyl)diethylenetriamine

溶媒

pyridine

pyridine

反応条件

後処理

1. 1
   その他transferred under warm conditions to an erlenmeyer flask
2. 2
   その他After returning to ambient temperature
3. 3
   workup.WAITThe mixture is left
4. 4
   workup.STIRRINGstirring overnight at ambient temperature
5. 5
   workup.WAITis then placed in an ice bath for 2 hours
6. 6
   ろ過The orange solid which then forms is filtered off
7. 7
   洗浄washed with cold (0° C.) 95% ethanol
8. 8
   その他After drying under vacuum at 40° C.
9. 9
   その他(rotary evaporator)

実験手順

115 g (0.6 mol) of p-toluenesulfonyl chloride are dissolved in 250 ml of pyridine at ambient temperature. A solution of diethylenetriamine (21.5 ml, 0.2 mol) in pyridine (30 ml) is added dropwise. The reaction mixture is stirred at 50° C. for 90 minutes and then transferred under warm conditions to an erlenmeyer flask. After returning to ambient temperature, 200 ml of water are added. The mixture is left stirring overnight at ambient temperature and is then placed in an ice bath for 2 hours. The orange solid which then forms is filtered off and washed with cold (0° C.) 95% ethanol. After drying under vacuum at 40° C. (rotary evaporator), the desired product is obtained in the form of a light yellow solid (92 g, yield 81%).

出典