Reacción #569002

Ecuación de reacción

butyllithium

2,2'-dibromobiphenyl

diethyl ether

hydrochloric acid

6-chloro-6H-dibenz[c,e][1,2]oxaphosphorine

→

2-(dibenzophosphol-9-yl)-2'-hydroxybiphenyl

Disolventes

hexane

o-xylene

water

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.STIRRINGThe mixture is then stirred for a further 2 hours at 25° C. and 3 hours at 50° C
2. 2
   TemperaturaThe mixture is cooled to room temperature
3. 3
   Otrothe organic phase is separated off
4. 4
   Secadodried with sodium sulfate
5. 5
   Concentraciónconcentrated under reduced pressure
6. 6
   OtroBy crystallization of the residue with 2-butanone, 11.8 g (90%) of colorless crystals
7. 7
   Otroare obtained

Procedimiento

46 ml of a 1.6M solution of butyllithium in hexane are added dropwise to a solution of 11.4 g (36.54 mmol) of 2,2'-dibromobiphenyl in 60 ml of diethyl ether. The mixture is then stirred for 24 hours at 20° C. To this is then added, at 0C, a solution of 8.6 g (36.5 mmol) of 6-chloro-6H-dibenz[c,e][1,2]oxaphosphorine in 30 ml of o-xylene. The mixture is then stirred for a further 2 hours at 25° C. and 3 hours at 50° C. The mixture is cooled to room temperature and 100 ml of water are carefully added. The mixture is neutralized with dilute hydrochloric acid, the organic phase is separated off, dried with sodium sulfate and concentrated under reduced pressure. By crystallization of the residue with 2-butanone, 11.8 g (90%) of colorless crystals having melting point 152° to 155° C. are obtained.

Fuente