in neat (no solvent)
Liquid N2O4 (- 4 °C) is dropped on PCl5 (- 18 °C); condensing of the red yellow vapor in a receiver cooled to - 20 °C; repetition of the reaction with the condensate;; rectification; pure product;;
in neat (no solvent)
distilling NO2 into an U-tube containing PCl5 at 24 °C; vigorous reaction; evolution of Cl2; collecting NOCl with receivers;; NOCl is impured with Cl2; fivefold distillation yield pure NOCl;;
