O-Xylene → 1-Chloro-2-fluoro-3-nitrobenzene

Participants

Reaction Conditions

Reaction Steps

In a 1-liter flange flask fitted with a distillation bridge and stirrer, 29 g (0.06 mol) of polyethylene glycol dimethyl ether 500 and 139 g (2.4 mol) of potassium fluoride were introduced at 120° C. into the melt of 576 g (3.0 mol) of 2,3-dichloronitrobenzene. Subsequently, 20 g (0.19 mol) of xylene were added and the reaction suspension was azeotropically dried by application of a vacuum of 60 mbar and heating to 150° C. After the xylene had been distilled off, the distillation bridge was replaced by a reflux condenser, the reaction suspension was heated to 190° C. and stirred for 6 hours at this temperature. Amount of 3-chloro-2-fluoronitrobenzene formed: 11 GC area-% after 6 hours.

Provenance & Evidence