Potassium Carbonate → Hexahydro-1-(3-methyl-4-nitrophenyl)-1H-1,4-diazepine

Participants

Reaction Conditions

Reaction Steps

Fluoronitrobenzene (9.1 g, 0.0586 mol) is dissolved in water (50 ml) and then potassium carbonate (9.7 9, 0.0703 mol) and 1-acetyl-[1,4]diazepane (10 g, 0.0703 mol) are added. The medium is heated at 95° C. for 6 hours, and an orange-coloured solution is obtained. The medium is then cooled to room temperature, and an orange-coloured sticky paste then appears. The maximum amount of water is removed from the reaction medium. Isopropanol is then added to the paste until a yellow solid precipitates. The medium is filtered and, after drying in a vacuum oven at 45° C., a yellow powder is obtained which corresponds to 1-(3-methyl-4-nitrophenyl)-[1,4]diazepane (1). (8.7 g; Yield=53.6%)

Provenance & Evidence