Hydrochloric Acid → HCID 6819364, compound

Participants

Reaction Steps

A suspension of 3.4-difluoroaniline (10 g, 0.0617 mol) in water (40 ml) and 37 per cent hydrochloric acid (5.3 ml, 0.064 mol) was added to a solution of chloral hydrate (11 g, 0.066 mol) and sodium sulfate (70 g) in water (240 ml). A solution of hydroxylamine hydrochloride (13.5 g, 0.195 mmol) in water (60 ml) was added to this mixture. The reaction mixture was boiled under reflux for 1 h, during which a clear reaction solution formed, from which are reaction product already precipitated out when hot. The mixture was stirred at room temperature for 16 h and, after filtration and washing with water (3×50 ml), the desired oxime was obtained in a yield of 91% (13.1 g) with a melting point of 179° C. as a yellow solid.

Provenance & Evidence