Pyridine → (4-Fluorophenyl)phosphonous dichloride

Temperature

73 °C

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.

1. customwas placed under an argon atmosphere in a 1 l flask
2. customwhich was provided with a thermostated jacket, mechanical stirring, thermometer
3. temperaturecooled to 60° C.
4. custommist was formed
5. stirringThe mixture was subsequently stirred for another 30 minutes at 60° C
6. customA nonuniform solid in the form of large lumps precipitated
7. customthis could not be separated off via a suction
8. filtrationfilter but only by filtration
9. washThe filtration residue was washed with petroleum ether
10. distillationdistilled

ORD record

ord-44d05bddb4ac4ff0867307918d01ee1e

Source dataset

uspto-grants-2010_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07767852B2