Phosphorus pentachloride → HCID 92004511, compound

Participants

Reaction Steps

To a rapidly stirring suspension of phosphorus pentachloride (150.0 g) in dry hexane (2.6 liters) is added 156.4 g (0.72 mole) of 7-chloro-2-nitroso-1-naphthol (VI). The mixture is stirred at room temperature for 1 hour after which it is refluxed for 2 hours. The hexane solution is decanted while hot, 2.0 liters of dry hexane are added to the residue in the flask, and refluxed for another hour. The hexane solution is decanted, combined with the first hexane extract and evaporated to dryness. Yield: 100 g, semi-solid dark brown residue. The crude product is extracted with 2.0 liters of hot dry hexane. The hot supernatant solution is decanted from the tarry residue at the bottom of the flask, concentrated to a volume of 700 ml and cooled in an ice bath. Repeated extractions of the original residue and tarry material are done with a total of 3.0 liters of hexane. All of the extracts are concentrated, cooled in an ice bath, and the product filtered off and dried. Total yield: 51.1 g (31.4%), mp 71°-74°.

Provenance & Evidence