Pyridine → (4-Fluorophenyl)phosphonous dichloride

Temperature

60 °C

A 1 l flask equipped with a thermostated jacket, mechanical stirring, thermometer and reflux condenser was initially charged under an argon atmosphere with a mixture of 3.4 mol of PCl3 and 1.2 mol of AlCl3 (98% purity) at 73° C. 0.8 mol of fluorobenzene was then added within 30 min, while a weak argon stream was passed through the reaction flask. The reaction mixture was stirred for 3 hours and cooled to 60° C., and 1.25 mol of pyridine were added slowly within 45 min. The reaction was exothermic and mist formed. Stirring was then continued at 60° C. for a further 30 min. An irregular, large-lumped solid precipitated which could not be removed via a suction filter, but only by filtration. The residue which was filtered off was washed with petroleum ether. The filtrate and washing liquid were combined and distilled to obtain 73.3 g of p-fluorophenyldichlorophosphine in a yield of 47% of theory.

1. customA 1 l flask equipped with a thermostated jacket, mechanical stirring
2. temperaturethermometer and reflux condenser
3. custommist formed
4. stirringStirring
5. waitwas then continued at 60° C. for a further 30 min
6. customAn irregular, large-lumped solid precipitated which could not
7. custombe removed via a suction
8. filtrationfilter
9. filtrationonly by filtration
10. filtrationThe residue which was filtered off
11. washwas washed with petroleum ether
12. washThe filtrate and washing liquid
13. distillationdistilled

ORD record

ord-e238337145c7482c9c9d51265af7417d

Source dataset

uspto-grants-2008_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07351339B2