Réaction #587223

Équation de réaction

pyridine

PCl3

AlCl3

fluorobenzene

→

p-fluorophenyldichlorophosphine

Rendement 47.0%

Conditions de réaction

Traitement

1. 1
   Autrewas placed under an argon atmosphere in a 1 l flask
2. 2
   Autrewhich was provided with a thermostated jacket, mechanical stirring, thermometer
3. 3
   Températurecooled to 60° C.
4. 4
   Autremist was formed
5. 5
   workup.STIRRINGThe mixture was subsequently stirred for another 30 minutes at 60° C
6. 6
   AutreA nonuniform solid in the form of large lumps precipitated
7. 7
   Autrethis could not be separated off via a suction
8. 8
   Filtrationfilter but only by filtration
9. 9
   LavageThe filtration residue was washed with petroleum ether
10. 10
    workup.DISTILLATIONdistilled

Mode opératoire

A mixture of 3.4 mol of PCl3 and 1.2 mol of AlCl3 (98% pure) was placed under an argon atmosphere in a 1 l flask which was provided with a thermostated jacket, mechanical stirring, thermometer and reflux condenser at 73° C. 0.8 mol of fluorobenzene was subsequently added over a period of 30 minutes, with a gentle stream of argon being passed through the reaction flask. The reaction mixture was stirred for 3 hours, cooled to 60° C. and 1.25 mol of pyridine were slowly added over a period of 45 minutes. The reaction was exothermic and mist was formed. The mixture was subsequently stirred for another 30 minutes at 60° C. A nonuniform solid in the form of large lumps precipitated, and this could not be separated off via a suction filter but only by filtration. The filtration residue was washed with petroleum ether. The filtrate and the washings were combined and distilled, giving 73.3 g of p-fluorophenyldichlorophosphine in a yield of 47% of theory.

Source