Water → HCID 178509230, compound

Participants

Reaction Steps

A suspension of 38.5 g (245.93 mmol) of 2-chloro-5-fluoronicotinonitrile was initially charged in 1,2-ethanediol (380 ml), and hydrazine hydrate (119.6 ml) was then added. With stirring, the mixture was heated at reflux for 4 h. Cooling resulted in the precipitation of a solid, which was admixed with water (380 ml) and extracted by stirring at RT for 10 min. The suspension was then filtered with suction through a frit, and the filter cake was washed with water (200 ml) and with THF at −10° C. (200 ml). The solid was dried under high vacuum over phosphorus pentoxide.

Provenance & Evidence