Methanol → N-ethyl-4-nitrobenzamide

Participants

Reaction Conditions

Reaction Steps

The reaction medium is reheated to 20° C. and 55 kg of methanol are then added. 24 kg (345 mol) of hydroxylamine hydrochloride are subsequently added and the reaction medium is heated to 45° C. 17 kg (207 mol) of sodium acetate are added and the heating is continued for 6 hours. The major portion of the solvents is removed by distillation under reduced pressure. The yellow-coloured reaction medium becomes viscous. 175 kg of distilled water are added at 65° C. The amidoxime gradually precipitates. The reaction medium is coloured orange/ochre. Stirring is continued at 45° C. for 1 hour. Filtering, rinsing with water and then drying results in 38.3 kg of the expected amidoxime, which is 98% pure as determined by TLC, signifying a yield of 77% based on the starting benzamide.

Provenance & Evidence