Reaktion #215548

Reaktionsgleichung

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

Lösungsmittel

toluene

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONis added dropwise in the course of 2 hours
2. 2
   Temperaturat reflux temperature for 4 hours
3. 3
   Sonstigetowards the end of the reaction, nitrogen gas
4. 4
   workup.ADDITIONis again introduced
5. 5
   workup.ADDITIONThere is then added dropwise
6. 6
   Temperaturat reflux temperature
7. 7
   Sonstige2 hours
8. 8
   Sonstigethe triethylamine hydrochloride which has precipitated
9. 9
   Filtrationis filtered off
10. 10
    SonstigeThe toluene is afterwards evaporated off

Vorschrift

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.

Quelle