反応 #215548

反応方程式

triethylamine

dibutylamine

4,4',6,6'-tetra-tert-butyl-2,2'-biphenol

phosphorus trichloride

→

N-(2,4,8,10-tetra-tert-butyl-dibenz[d,f][1,3,2]dioxaphosphepin-6-yl)-dibutylamine

溶媒

toluene

toluene

反応条件

後処理

1. 1
   workup.ADDITIONis added dropwise in the course of 2 hours
2. 2
   温度at reflux temperature for 4 hours
3. 3
   その他towards the end of the reaction, nitrogen gas
4. 4
   workup.ADDITIONis again introduced
5. 5
   workup.ADDITIONThere is then added dropwise
6. 6
   温度at reflux temperature
7. 7
   その他2 hours
8. 8
   その他the triethylamine hydrochloride which has precipitated
9. 9
   ろ過is filtered off
10. 10
    その他The toluene is afterwards evaporated off

実験手順

170 g (0.414 mol) of 4,4',6,6'-tetra-tert-butyl-2,2'-biphenol in 150 ml of toluene is heated to 80°-90° C. in a nitrogen atmosphere, and 40 ml (0.458 mol) of phosphorus trichloride is added dropwise in the course of 2 hours. The reaction mixture is stirred at reflux temperature for 4 hours and, towards the end of the reaction, nitrogen gas is again introduced. There is then added dropwise at reflux temperature, during 11/2 hours, a solution of 53.5 g (0.414 mol) of dibutylamine and 41.9 g (0.414 mol) of triethylamine in 80 ml of toluene. After 15 hours, the reaction mixture is allowed to cool to room temperature, and the triethylamine hydrochloride which has precipitated is filtered off. The toluene is afterwards evaporated off, and the N-(2,4,8,10-tetra-tert-butyl-dibenz[d,f][1,3,2]dioxaphosphepin-6-yl)-dibutylamine obtained has a melting point of 140° C.

出典