Benzene → HCID 18988728, compound

Participants

Reaction Steps

A solution of 3,5-dinitrobenzoyl chloride (50.00 g, 0.22 mol), freshly distilled ε-caprolactam (24.54 g, 0.22 mol) and 500 ml of benzene is added to a 1L, three-necked, round-bottom flask equipped with an overhead stirrer, condenser and a nitrogen inlet tube. The solution is heated to 90°-100° C. After all the solids are dissolved, 165 ml of pyridine is added. White pyridine salts form immediately, and the reaction solution is kept at 90°-100° C. for 1 hour before removing the pyridine salts by filtration. The solvent is removed from the filtrate under reduced pressure and the residue is washed by a 5 percent NaHCO3 aqueous solution and distilled water several times before being dried. The product is recrystallized from a mixture of ethyl acetate and hexane to obtain 45 g (68 percent) of white crystals: mp 126°-126.5° .

Provenance & Evidence