반응 #215548

반응 방정식

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

용매

toluene

toluene

반응 조건

후처리

1. 1
   workup.ADDITIONis added dropwise in the course of 2 hours
2. 2
   온도at reflux temperature for 4 hours
3. 3
   기타towards the end of the reaction, nitrogen gas
4. 4
   workup.ADDITIONis again introduced
5. 5
   workup.ADDITIONThere is then added dropwise
6. 6
   온도at reflux temperature
7. 7
   기타2 hours
8. 8
   기타the triethylamine hydrochloride which has precipitated
9. 9
   여과is filtered off
10. 10
    기타The toluene is afterwards evaporated off

실험 절차

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.

출처